Parallel reactor for sampling and conducting in situ flow-through reactions and a method of using same

ABSTRACT

An apparatus for parallel processing of reaction mixtures, including a reactor block including reaction chambers for containing reaction mixtures under pressure, the reactor block further including a first sidewall, a second sidewall, and a first plurality of fluid flow paths providing fluid communication with the first sidewall and respective reaction chambers and the second sidewall and respective reaction chambers;; a stirring system including a base plate defining a second plurality of flow paths, wherein respective flow paths of said second plurality of flow paths are in fluid communication with respective reaction chambers and respective fluid flow paths of said first plurality of flow paths, and the base plate also supports a plurality of stirring blade assemblies for mixing the reaction mixtures; interchangeable manifolds supported by the first sidewall and the second sidewall, the interchangeable manifolds defining a plurality of manifold inlet/outlet ports, wherein respective inlet/outlet ports of said plurality of inlet/outlet ports are in communication with respective fluid flow paths of said first plurality of fluid flow paths and permit fluid to be introduced into or vented from the respective reaction chambers; and a sampling manifold assembly coupled in fluid communication with the respective reaction chambers, wherein a portion of the reaction mixture retained in the respective reaction chambers can be withdrawn from the respective reaction chamber through respective fluid flow paths of said first plurality of fluid flow paths and respective flow paths of said second plurality of flow paths, or both, without depressurizing or lowering the pressure in the respective reaction chamber.

FIELD OF THE INVENTION

[0001] The present invention relates to an apparatus and method forcarrying out and in situ monitoring of the progress and properties ofmultiple parallel reactions.

BACKGROUND OF THE INVENTION

[0002] In combinatorial chemistry, a large number of candidate materialsare created from a relatively small set of precursors and subsequentlyevaluated for suitability for a particular application. As currentlypracticed, combinatorial chemistry permits scientists to systematicallyexplore the influence of structural variations in candidates bydramatically accelerating the rates at which they are created andevaluated. Compared to traditional discovery methods, combinatorialmethods sharply reduce the costs associated with preparing and screeningeach candidate.

[0003] Combinatorial chemistry has revolutionized the process of drugdiscovery. One can view drug discovery as a two-step process: acquiringcandidate compounds through laboratory synthesis or through naturalproducts collection, followed by evaluation or screening for efficacy.Pharmaceutical researchers have long used high-throughput screening(HTS) protocols to rapidly evaluate the therapeutic value of naturalproducts and libraries of compounds synthesized and cataloged over manyyears. However, compared to HTS protocols, chemical synthesis hashistorically been a slow, arduous process. With the advent ofcombinatorial methods, scientists can now create large libraries oforganic molecules at a pace on par with HTS protocols.

[0004] Recently, combinatorial approaches have been used for discoveryprograms unrelated to drugs. For example, some researchers haverecognized that combinatorial strategies also offer promise for thediscovery of inorganic compounds such as high-temperaturesuperconductors, magnetoresistive materials, luminescent materials, andcatalytic materials. See, for example, co-pending U.S. patentapplication Ser. No. 08/327,513 “The Combinatorial Synthesis of NovelMaterials” (published as WO 96/11878) and co-pending U.S. patentapplication Ser. No. 08/898,715 “Combinatorial Synthesis and Analysis ofOrganometallic Compounds and Catalysts” (published, in part, as WO98/03251), which are all herein incorporated by reference.

[0005] Because of the success of the combinatorial approach ineliminating the synthesis bottleneck in drug discovery, many researchershave come to narrowly view combinatorial methods as tools for creatingstructural diversity. Few researchers have emphasized that, duringsynthesis, variations in temperature, pressure, ionic strength, andother process conditions can strongly influence the properties oflibrary members. For instance, reaction conditions are particularlyimportant in formulation chemistry, where one combines a set ofcomponents under different reaction conditions or concentrations todetermine their influence on product properties.

[0006] In recent years, researchers have begun to design apparatus to beused in combinatorial experiments that allow parallel processing ofmultiple reactions, particularly where it is desirable to vary one ormore parameters of the reactions. For instance, commonly assignedpending U.S. application Ser. No. 09/548,848 filed on Apr. 13, 2000,discloses a parallel reactor including vessels for containing aplurality of reaction mixtures, a stirring system, and a temperaturecontrol system adapted to maintain the individual vessels or groups ofvessels at different temperatures. The Ser. No. 09/548,848 applicationis a continuation-in-part of pending U.S. application Ser. Nos.09/239,223 and 09/211,982 filed Jan. 29, 1999 and Dec. 14, 1998,respectively, wherein the Ser. No. 09/211,982 application is acontinuation-in-part of pending U.S. Ser. No. 09/177,170 filed on Oct.22, 1998, which is itself a continuation-in-part of ProvisionalApplication No. 60/096,603 filed Aug. 13, 1998, now abandoned, all ofwhich are incorporated herein by reference.

[0007] Commonly assigned pending Provisional Application Ser. No.60/255,716 filed on Dec. 14, 2000, incorporated herein by reference,also describes a related apparatus. In particular Application No.60/255,716 discloses parallel semi-continuous or continuous reactors forsynthesizing combinatorial libraries of materials and screeningcombinatorial libraries of materials such as catalysts.

[0008] Given the growing interest in combinatorial research, it may bedesirable to have a parallel reactor adapted to create various flowpaths through the reactor block while allowing in situ monitoring andcontrol over the progress and properties of multiple parallel reactions,as well as permit the removal of a portion of the reaction mixturesduring the experiment or the performance of flow-through experiments,wherein both sampling and flow-through can occur without depressurizingor reducing the pressure in the respective reaction chambers.

SUMMARY OF THE INVENTION

[0009] The present invention relates to an apparatus and method forcarrying out and in situ monitoring multiple parallel reactions.Specifically, the apparatus can be used for making, characterizing andsampling reaction mixtures, and can include a reactor block, reactionchambers, a stirring system, interchangeable manifolds and a samplingmanifold assembly.

[0010] The reactor block can include reaction chambers for containingreaction mixtures under pressure. The reactor block can further includea first sidewall, a second sidewall, and a first plurality of fluid flowpaths providing fluid communication with the first sidewall andrespective reaction chambers and the second sidewall and respectivereaction chambers.

[0011] In a preferred embodiment the, first and second plurality of flowpaths are channels formed through the reactor block and the base plateof the stirring system, respectively, and a group of four fluid flowpaths from the first plurality of fluid flow paths are in fluidcommunication with a single reaction chamber. More specifically, two ofthe four fluid flow paths are defined by the first sidewall and two ofthe four fluid flow paths are defined by the second sidewall. And evenmore specifically, one of the two fluid flow paths defined by the firstsidewall is in fluid communication with a respective reaction chamberreaction chamber via a respective flow path from the second plurality offlow paths, and one of the two fluid flow paths defined by the secondsidewall is in fluid communication with a respective reaction chambervia one flow path of the second plurality of flow paths.

[0012] The stirring system can include a base plate defining a secondplurality of flow paths. At least one flow path of the second pluralityof flow paths is in fluid communication with respective reactionchambers, at least one fluid flow path of the first plurality of flowpaths. The base plate supporting a plurality of stirring bladeassemblies for mixing the reaction mixtures, wherein one stirring bladeassembly of the plurality of stirring blade assemblies is received inthe respective reaction chambers.

[0013] The interchangeable manifolds can be supported by the firstsidewall and the second sidewall, and can define a plurality of manifoldinlet/outlet ports. Each respective inlet/outlet port of the pluralityof inlet/outlet ports is in communication with respective fluid flowpaths of the first plurality of fluid flow paths and permits fluid to beintroduced into or vented from the respective reaction chambers.

[0014] The interchangeable manifolds allow the first and secondplurality of flow paths to be coupled in a variety of configurations.For instance, the plurality of inlet/outlet ports of the interchangeablemanifold bars can define separate flow paths through the respectiveinterchangeable manifold bars which align with respective flow pathsthrough the reactor block or the base plate, respectively. For instance,a first group of inlet/outlet ports of the plurality of inlet/outletports can include inlet/outlet ports placed in fluid communication withrespective flow paths of the first plurality of flow paths andrespective flow paths of the second plurality of flow paths, whereineach inlet/outlet port of the first group is in fluid communication withrespective flow paths of the first plurality of fluid flow paths andwith respective flow paths of the second plurality of fluid flow paths.And, a second group of inlet/outlet ports selected from the plurality ofinlet/outlet ports can be placed in fluid communication with respectiveflow paths of the first plurality of fluid flow paths, wherein therespective flow paths of the first plurality of fluid flow paths is influid communication with a head space defined within the respectivereaction chambers, and wherein each inlet/outlet port of the secondgroup is in fluid communication with a respective flow path of the firstplurality of fluid flow paths.

[0015] Alternatively, the interchangeable manifolds can be set up toinclude a fifth group of inlet/outlet ports selected from the pluralityof inlet/outlet ports. The inlet/outlet ports forming the fifth groupare coupled in fluid communication so as to define a common flow paththrough the fifth group such that each inlet/outlet port of the fifthgroup is in fluid communication with separate flow paths forming thefirst plurality of fluid flow paths. Thus, each inlet/outlet port ofthis fifth group of inlet/outlet ports can be coupled to a common fluidor pressure source. Additionally, each inlet/outlet port of the fifthgroup of inlet/outlet ports can be placed in fluid communication withthe respective reaction chambers.

[0016] In another embodiment, the parallel reactor can include asampling manifold for allowing a sample to be withdrawn from thereaction chambers without depressurizing the reaction chamber orreducing the pressure in the reaction chamber. In a preferredembodiment, the sampling manifold assembly is coupled in fluidcommunication with the respective reaction chambers via at least oneinterchangeable manifold. For instance, a portion of the reactionmixture retained in the respective reaction chambers can be withdrawnfrom the respective reaction chamber through respective fluid flow pathsof the first plurality of fluid flow paths and respective flow paths ofthe second plurality of flow paths, or both, without depressurizing orlowering the pressure in the respective reaction chamber.

[0017] A method of processing multiple reaction mixtures using thereactor 10 in can include the steps of (1) providing interchangeablemanifolds having inlet/outlet ports in fluid communication with therespective reaction chambers, wherein a fluid can be introduced into orwithdrawn from the respective reaction chambers; and (2) evaluating oneor more properties of the reaction mixtures or a portion of the reactionmixture by measuring at least one characteristic of the reactionmixtures during at least a portion of the reaction. Additionally, themethod could include the step of sampling a portion of the reactionmixture from the respective reaction chambers via at least one of theinterchangeable manifolds, wherein sampling occurs at a pressure greaterthan ambient conditions and without reducing the pressure in therespective reaction chambers. And the step of providing the reactionchambers with starting mixtures can be performed by a robotic materialshandling system or the starting materials could be manually added to therespective reaction chambers.

BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The features and inventive aspects of the present invention willbecome more apparent upon reading the following detailed description,claims, and drawings, of which the following is a brief description:

[0019]FIG. 1 shows a perspective view of a parallel reactor assemblyformed in accordance with the teachings of the present invention.

[0020]FIGS. 2a-d show a rear, top and side view of the parallel reactorblock assembly shown in FIG. 1.

[0021]FIGS. 3a-d show a front perspective view and a detailed view ofthe reactor block shown in FIG. 1.

[0022]FIG. 4 shows a rear perspective view of the parallel reactor blockassembly shown in FIG. 1.

[0023]FIG. 5 shows a section view of one reactor well (reaction chamber)of the parallel reactor shown in FIG. 1.

[0024]FIG. 6 shows a section view of the parallel reactor shown in FIG.2a taken along the line 6-6.

[0025]FIG. 7 is a detail view of the structure shown in FIG. 6, showingthe internal flow paths through the parallel reactor.

[0026]FIG. 8 shows a perspective view of a stir top assembly that formspart of the parallel reactor shown in FIG. 1.

[0027]FIG. 9 shows a bottom perspective view of the stir top assemblyshown in FIG. 8.

[0028]FIG. 10 shows an alternative embodiment of a stir top assemblyformed in accordance with the teachings of this invention.

[0029]FIG. 11 shows a perspective view of the exterior and interior ofthe heater and motor control box shown in FIG. 1.

[0030]FIG. 12 shows a perspective view of a sampling manifold assemblythat forms a part of the parallel reactor shown in FIG. 1.

[0031]FIG. 13 shows a rear perspective of the sampling manifold shown inFIG. 12, and illustrates the manner in which the flow valves shown inFIG. 12 are coupled to the sampling manifold plate.

[0032]FIG. 14 shows a rear perspective view of the sampling manifoldassembly shown in FIG. 12.

[0033]FIG. 15 shows a schematic diagram showing a single flow paththrough the sampling manifold assembly shown in FIG. 12.

[0034]FIGS. 16a-b show a perspective view of a general use manifoldassembly formed in accordance with the teachings of this invention.

[0035]FIGS. 17a-b show a perspective view of a flow-through manifoldassembly formed in accordance with the teachings of this invention.

[0036]FIGS. 18a-b show a perspective view of a static pressure manifoldassembly formed in accordance with the teachings of this invention.

[0037]FIG. 19 shows a materials handling robotic systems used to addstarting materials to the reaction chambers.

[0038]FIG. 20 shows an alternative embodiment of the parallel reactorshown in FIG. 1, wherein a sampling manifold establishes direct fluidcommunication with the reaction chambers.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

[0039] The present invention is described herein with reference to theaccompanying figures. Terms of reference such as “top” and “bottom” areused to facilitate an understanding of the present invention in view ofthe accompanying figures. The identified reference terms or othersimilar terms are not intended to be limiting, and one of ordinary skillin the art will recognize that the present invention can be practiced ina variety of spatial orientations without departing from the spirit andscope of the invention.

[0040] The apparatus comprising the present invention is particularlyuseful for the research and development of chemical reactions, catalystsand processes, and is especially useful for synthesizing, screening, andcharacterizing combinatorial libraries. The present invention providesan apparatus and method for carrying out and monitoring the progress andproperties of multiple reactions in situ, and includes a reaction blockassembly defining multiple reaction chambers.

[0041] The apparatus offers significant advantages over conventionalexperimental reactors. For example, the apparatus can provide in situsampling of individual reaction mixtures and in situ injection ofadditional chemistry or components into one or more reaction chambers.Both in situ sampling and the injection of chemistry or other componentscan occur without depressurizing or lowering the pressure in therespective reaction chambers.

[0042] The present invention also permits the performance offlow-through experimentation, wherein flow-through experimentation cantake place at pressures greater than atmospheric pressure, with an upperlimit preferably set at 1500 psi. The present invention also permitscontinuous or semi-continuous flow-through experimentation.

[0043] Another advantage of the present invention is the ability tointerchange manifold assemblies coupled to the reactor assembly so as tocreate various flow paths and flow patterns through the reactor block.The interchangeable manifolds permit opposing sides of the reactor blockto be set up having identical or different flow path configurations.

[0044] Other advantages of the present invention result from the use ofsmall volume mixtures. In addition to conserving valuable reactionmixtures, decreasing sample size increases surface area relative tovolume within individual reaction chambers. This improves the uniformityof reaction mixtures, aids gas-liquid exchange in multiphase reactions,and increases heat transfer between the samples and the respectivereaction chambers. Because large samples respond much slower to changesin system conditions, the use of small samples, along with in situmonitoring and process control, also allows for time-dependentprocessing and characterization.

Overview of Parallel Reactor

[0045] The parallel reactor system of the present invention is a modularplatform for effecting combinatorial research in chemistry and materialsscience applications. Although the parallel reactor system of thepresent invention is designed to be a modular unit, the parallel reactorsystem can be designed for integration into a larger screening device asdisclosed in commonly assigned U.S. application Ser. No. 09/548,848, thediscussion of which is incorporated herein by reference.

[0046] The parallel reactor includes a plurality of reaction chambersthat can be operated in parallel on a scale suitable for researchapplications, typically bench scale or smaller scale (e.g.,mini-reactors and micro-reactors). The reaction chambers of the parallelreactor can typically, but not necessarily, be formed in, be integralwith or be linked by a common substrate, be arranged in a common plane,preferably with spatial uniformity, and/or can share a common supportstructure or housing.

[0047] The same or different reactions (experiments) may be performed ineach well. Thus, each reactor well may vary with regard to its contentsduring an experiment. Each reactor well can also vary by a processcondition, including catalyst amounts (volume, moles or mass), ratios ofstarting components, time for reaction, reaction temperature, reactionpressure, rate of reactant addition to the reaction, reactionatmosphere, injection of a catalyst or reactant or other component(e.g., a reaction quencher) and other conditions that those of skill inthe art will recognize. Each reaction chamber can also vary by thechemicals present, such as by using different reaction mixtures orcatalysts in two or more reaction chambers.

[0048] The parallel reactor is also designed to permit separateagitation of each sample by stirring the reaction mixtures in therespective well at selected times during the experiment withoutdepressurizing or lower the pressure of the reactor well. The parallelreactor also permits the injection of additional chemistry into adesired well at selected times during the experiment. Further still, theparallel reactor is designed to allow the real-time collection ofsamples under pressure from each well at any time during an experiment.Finally, the parallel reactor also permits the performance offlow-through reactions continuously or at selected times during theexperiment.

[0049]FIG. 1 shows one embodiment of a parallel reactor system 10 formedin accordance with the teachings of this invention. The reactor system10 can include a reactor block assembly 12, a stir top assembly 26, amanifold assembly 56, a sampling manifold assembly 58, and a heater andmotor control box 116.

[0050] The Reactor Block

[0051] FIGS. 1-4 show a reactor block 12 formed in accordance with theteachings of this invention. As best seen in FIGS. 3a-d, the reactorblock 12 includes a rectangularly shaped body including a top surface 22a, opposing sidewall surfaces 22 b, 22 b′ and opposing end surfaces 22c. The reactor block 12 can be fabricated using a metal,glass/quartz/ceramic or plastic material. Preferably, the reactor block12 is fabricated of stainless steel; however, one of skill in the artwill appreciate that materials having similar chemical or mechanicalproperties could be used. One of skill in the art will also appreciatethat the reactor block 12 can be formed using other configurations orshapes.

[0052] The reactor block 12 defines a plurality of reaction chambers inthe form of reactor wells 14 for receiving and retaining the reactionmixtures. As best illustrated in FIGS. 3a-c and 4, the reactor block 12defines eight reactor wells 14 formed in the reactor block 12 usingknown machining or metal working techniques. One of skill in the artwill appreciate that the reactor block 12 could be designed to includeany desired number of reactor wells 14.

[0053] Each well 14 defines a rectangularly shaped body 14 a thatprojects downwardly from the top surface 22 a. Each body 14 a isseparated from an adjacent body 14 a by an air gap such that eachreactor well 14 defines a separate reaction chamber that can be used toperform the same or different experiments in parallel. The air gap alsothermally isolates adjacent well bodies 14 a, which helps improve theefficiency of the parallel reactor system 10.

[0054] Referring back now to FIGS. 2c and 6, the bottom surface 140 ofthe well body 14 a is coupled to a pressure control valve 15. In thedisclosed embodiment, the surface 140 supports threads for mating with astandard burst disk supporting mating threads, as best seen in FIG. 6.One of skill in the art will appreciate that other types of pressurecontrol devices could be used, and that other known methods can be usedto install such devices.

[0055] Referring now to FIGS. 3a, b and 6, each reactor well body 14 aincludes an open center 14 b. The open center 14 b can extend downwardlythrough at least a portion of the body 14 a. As shown in FIG. 3a, theopen center 14 b can originate at the top surface 22 a, wherein it issurrounded by an O-ring interface 13, and continue through the body 14 aterminating at the bottom surface 140.

[0056] The open centers 14 b can be sized such that the volume retainedby each reactor well 14 can be the same or different. The volume of eachreactor well 14 may vary from about 0.1 milliliter (ml) to about 500 ml,more particularly from about 1 ml to about 100 ml and even moreparticularly from about 5 ml to about 20 ml. These well 14 sizes allowfor reaction mixture volumes in a range that functionally allow forproper agitation of the sample by stirring (e.g., a 15 ml reactor vesselallows for reactant volumes of between about 2-10 ml). Also, theparallel reactor 10 allows the pressure to vary from reactor well 14 toreactor well 14, with each reactor well 14 being pressurized to apositive pressure, wherein the upper pressure limit can be equal to orgreater than 1500 psi, with the preferred upper limit set at 1500 psi.Additionally, the reactor temperature can vary from reactor well 14 toreactor well 14, with each reactor well 14 generally operating at amaximum temperature of about 250° C. In will be appreciated that thereactor 10 could be designed to operate at temperatures and pressuresabove or below the aforementioned values.

[0057] As shown in FIGS. 2a and 5, each open center 14 b can receive andsupport a closed bottom removable vessel 16 into which the reactionmixtures can be received. As best seen in FIGS. 2a and 5, the vessels 16can include a diameter sized to be received within each of therespective reactor wells 14, and, preferably, the closed bottom of thevessel 16 is continuous with the bottom surface 140 of the well body 14a.

[0058] The vessels 16 can include a length that is shorter than thelength of the reactor well 14, as best seen in FIG. 5. As a result, theupper end of the removable vessels 16 is not contiguous with the topsurface of the well 14, since the top surface of the reactor wellterminates at the top surface 22 a. This arrangement defines a headspace 17 above the vessels 16 (or the reaction mixture) that allowsmixing or stirring the reaction mixtures within the well 14/vessel 16.

[0059] When using the removable vessels 16, one can select vessels 16made of a material appropriate for a given set of reaction mixtures,products, and reaction conditions. For instance, the removable vessels16 can be glass, plastic or Teflon® test tubes or vials sized so that avessel 16 fits within the open center 14 b of a single reactor well 14.The removable vessels 16 can also be liners fabricated of a polymermaterial, wherein the liners cover at least a portion of the open centerof the respective reactor wells 14, providing a protective covering overat least a portion of the interior surface of the reactor well 14.

[0060] Although the reaction mixtures could be received directly by thewell 14 in the respective openings 14 b, the removable vessels 16 canprovide several advantages. For example, the vessels 16 prevent thereaction mixtures from coming into direct contact with the reactionblock 12, as such contact could be the source of contaminants insubsequent experiments. Unlike the reactor block 12, which represents asignificant investment, the vessels 16 can be discarded if damaged afteruse. Furthermore, the vessels 16 permit removal of one or more vessels16 from the reactor block 12 for further in-depth characterization atvarious times during the experiment. Finally, one can lower materialcosts and ensure compatibility with standardized sample preparation andtesting equipment by designing the reactor block 12 to accommodatecommercially available vessels 16.

[0061] In addition to the reactor wells 14, the reactor block 12 isconfigured to support or retain various components. Referring to the topsurface 22 a as shown in FIGS. 3a-d, the top surface 22 a defines aplurality of mounting holes 11 a along a portion of the length thereoffor receiving threaded fasteners such as screws or bolts. The topsurface 22 a also defines one or more smaller openings 11 b forreceiving a locating pin, for example, a dowel pin for aligning thereactor block 12 with a mating component. As best seen in FIGS. 3a, 4,the openings 11 b can be centrally located at opposite ends of thereactor block 12 along the width of the surface 22 a.

[0062]FIG. 4 also shows a pair of openings 27. The openings 27 areformed along opposing edges of the top surface 22 a using knownmachining techniques such that openings 27 are in fluid communicationwith respective paths 20 a, 20 b (discussed in more detail below). Asbest seen in FIG. 3b, each opening 27 is surrounded by a respectiveO-ring interface 27 a, 27 b, wherein the O-ring interfaces 27 a, 27 bare formed in the surface 22 a using known machining or metal workingtechniques.

[0063] Referring now to FIGS. 3a and 4, the opposing end surfaces 22 care substantially planar and include a plurality of threaded openingsfor receiving threaded fasteners such as bolts or screws. Each endsurface 22 c supports a leg 18, as best seen in FIGS. 1, 2a, 2 c and 4.

[0064] As shown in FIG. 2c, each leg 18 is a rectangularly shapedmember, and defines an open center 18 c that extends along a portion ofthe length of the leg 18, a first end 18 a and a second end 18 b. Itwill be appreciated that the leg 18 can be configured having a differentgeometrical shape.

[0065] The first end 18 a includes a substantially planar solid surfacethat includes a plurality of openings for receiving threaded fasteners.The first end 18 a acts as a mounting bracket for coupling the leg 18 tothe reactor block at the opposing ends 22 c. As best seen in FIG. 4, thelegs 18 can be coupled to the opposing ends 22 c by inserting threadedfasteners into aligned threaded openings defined by both the ends 22 cand the legs 18. Alternatively, the legs 18 could be integrally formedwith the end surfaces 22 c or coupled to the end surfaces 22 c usingwelding techniques or other similar methods.

[0066] The open center 18 c of each leg 18 is contiguous with the firstend 18 a and extends through the leg 18 to the second end 18 b. At thesecond end 18 b the leg 18 defines a triangularly shaped surface area 18d that projects outwardly from the second end 18 b. The triangularlyshaped surface area 18 d defines a foot upon which the leg 18 stands.Each leg 18, particularly the triangularly-shaped surface area 18 c, isconfigured to impart stability to the reactor block 12, allowing thereactor block 12 to stand alone independent of other supporting devices.Alternatively, the foot includes openings 138 for receiving fastenerssuch as screws or bolts for coupling the leg 18 to a mating component.

[0067] As best seen in FIG. 4, one leg 18 supports a motor 19. The motor19 can be coupled to the leg 18 via a standard mounting bracket 19 busing threaded fasteners or other similar devices, wherein the mountingbracket 19 b includes a closed sidewall surface and an open top andbottom. Also, as best seen in FIG. 4, the motor 19 includes an outwardlyextending motor shaft 19 a. In the disclosed embodiment, the motor 19 isa brushless AC drive motor, although other types of motors could be usedsuch as an air-driven motor, a DC stepper motor or other known AC or DCmotors, including variable or constant speed motors.

[0068] Turning now to a discussion of the opposing sidewall surfaces 22b, 22 b′, as best seen in FIGS. 3a-d, each opposing sidewall surface 22b, 22 b′ defines a plurality of threaded holes 23 along the length ofthe sidewall surface 22 b, 22 b′ for receiving threaded fasteners.Additionally, each sidewall surface 22 b, 22 b′ defines an opening 20 asbest seen in FIG. 3d. Each opening 20 can be machined in the respectivesidewall 22 b, 22 b′ using known machining techniques, and is configuredto permit passage of a fluid, wherein the fluid can be either a liquidor gas, through though the sidewall 22 b, 22 b′, respectively.

[0069] As best seen in FIG. 7, each opening 20 is in fluid communicationwith a separate fluid flow path 20 a, 20 b defined through the reactorblock 12 through the respective sidewalls 22 b, 22 b. And each fluidflow path 20 a, 20 b establishes fluid communication with a respectivewell 14, as will be described in more detail below. In the embodimentshown in FIG. 7, each flow path 20 a, 20 b extends through a portion ofthe respective sidewall surface 22 b, 22 b′ in the direction of the well14. However, prior to intersecting the well 14, each flow path 20 a, 20b turns approximately 90° and terminates at the top surface 22 aadjacent a respective opening 27, as shown in FIGS. 5 and 7. Thisarrangement establishes fluid flow paths 20 a, 20 b through at lest aportion of the respective sidewall surface 22 b, 22 b′.

[0070] Each flow path 20 a, 20 b can be formed through the respectivesidewall 22 b, 22 b′ using knowing machining techniques. And it will beappreciated that the flow paths 20 a, 20 b could be machined so as toextend through the entire width of the respective sidewall 22 b, 22 b′and caused to provide fluid communication directly with the well 14 asshown by the phantom lines in FIG. 5. Furthermore, it will beappreciated that other known techniques could be used to establish therespective flow paths 20 a, 20 b through the reactor block 12.

[0071] Referring back to FIGS. 3d and 7, each sidewall surface 22 b, 22b′ defines a second opening 21 positioned vertically below the opening20. Each opening 21 can be machined in the respective sidewall 22 b, 22b′ using known machining techniques. It will be appreciated that othertechniques could be used to form each opening 21.

[0072] Each opening 21 is adapted to permit the passage of a fluid,preferably a gas, through the respective sidewall 22 b, 22 b′,consequently, the opening 21 is also referenced to as a gas port. Asbest seen in FIG. 7, each opening 21 is in fluid communication withseparate fluid flow paths 21 a, 21 b defined through the reactor block12 through the respective sidewall surfaces 22 b, 22 b′. The pair offluid flow paths 21 a, 21 b can be machined through the respectivesidewall surface 22 b, 22 b′ using known techniques, and caused toterminate at opposite sides of the inner surface of a single reactorwell 14, as best shown in FIGS. 5 and 7. This arrangement not onlyresults in the terminal end of each flow path 21 a, 21 b being in fluidcommunication with opposite sides of the interior of a respective well14, this arrangement establishes fluid communication between each flowpath 21 a, 21 b and the head space 17, as best seen in FIG. 5.Consequently, each flow path 21 a, 21 b can be separately vented to thehead space 17.

[0073] Reactor Block Manifold Assemblies

[0074] The reactor block manifold assemblies allow one or more fluids,liquid or gas, to be introduced into, withdrawn from or vented throughthe reactor wells 14. For instance, the reactor block manifoldassemblies can include fluid flow paths that provide fluid communicationbetween the respective wells 14 and the manifold assembly. The manifoldflow paths can be configured to permit selective control over the mannerin which fluid is introduced into, withdrawn from or vented through thewells 14. For instance, each inlet/outlet port of the manifoldassemblies can be separately coupled to a respective well 14 and one ormore fluid sources, the inlet/outlet ports can be coupled to therespective wells 14 so as to create a common flow path to one or more ofthe wells 14, or certain flow paths can be plugged to prevent flowthrough the respective flow path. Even further still, the reactor blockmanifold assemblies can include components such as check valves or otherflow control valves that permit selective control over the fluid flowpaths between a particular manifold assembly and the respective wells14.

[0075] As best seen in FIG. 4, the reactor block 12 can support ageneral use manifold assembly 56 to establish a variety of fluid flowpatterns through the reactor block 12. The manifold assembly 56 caninclude a pair of metal elongated bars 55, the bars preferably beingstainless steel.

[0076] As best seen in FIGS. 4 and 16b, each manifold bar 55 can beidentically formed so as to include a plurality of axially alignedinlet/outlet port pairs 53 a, 53 b formed along the length thereof. Asshown in FIGS. 7 and 16a, b, the manifold bar 55 includes sixteenseparate inlet/outlet ports 53 a, 53 b, each inlet/outlet port 53 a, 53b establishing a flow path through the manifold bar 55.

[0077] As best seen in FIG. 7, the inlet/outlet ports 53 a, 53 b cansupport a standard fitting (not shown), and can be sized and configuredto receive a conduit or other vessel for transferring fluids into or outof the separate wells 14 or vessels 16. Each inlet/outlet port pair 53a, 53 b is surrounded by an O-ring interface 53 a′, 53 b′, respectively.As best seen in FIG. 7, O-ring interface 53 a′ is associated withinlet/outlet port 53 a, and O-ring interface 53 b′ is associated withinlet/outlet port 53 b. It will be appreciated that openings 53 a, 53 band O-ring interfaces 53 a′, 53 b′ can be formed in the manifold bar 55using known machining or metal working techniques.

[0078] Referring back to FIGS. 4 and 16b, the manifold bar 55 can alsoinclude a plurality of openings 57 for receiving threaded fasteners suchas screws or bolts for coupling the respective manifold bar to thereactor block 12. As shown in FIG. 7, each manifold bar 55 is supportedby the respective sidewall surface 22 b, 22 b′ such that separatemanifold inlet/outlet ports 53 a, 53 b align with and are in fluidcommunication with respective openings 20 and 21. This arrangementpermits fluid communication between respective inlet/outlet ports 53 a,53 b and a single well 14.

[0079] As best seen in FIG. 7, when a manifold bar 55 is coupled to thereactor block 12 at sidewall 22 b, each inlet/outlet port 53 a, 53 b isplaced in fluid communication with respective openings 20 and 21 so asto establish fluid communication with respective flow paths 20 a, 21 a.And if a second manifold bar 55 is coupled to sidewall 22 b′, eachinlet/outlet port 53 a, 53 b is placed in fluid communication withrespective openings 20 and 21 so as to establish fluid communicationwith respective flow paths 20 b, 21 b. This arrangement permits separatefluid flow paths to be established through each of flow path 20 a, 20 b,21 a, and 21 b.

[0080] While the general use manifold 56 provides great flexibility inhow the reactor block 12 can be configured to receive or vent fluids,the general manifold 56 requires the use of at least 32 lines orconnections to establish fluid communication between each of the 32manifold inlet/outlet ports 53 a, 53 b and each respective opening 20,21.

[0081] Flow-Through Manifold

[0082] In another embodiment, the general use manifold assembly 56 canbe configured as a flow-through manifold 600, as shown in FIGS. 17a, b.It will be appreciated that the general use manifold assembly 56 and theflow-through manifold 600 share common elements. Thus, common referencenumerals are used to describe common features. Flow-through occurs whena fluid, preferably a gas, is received in one or more reactor wells 14through the respective flow paths 20 a, 20 b and vented out through oneor more other inlet/outlet ports in fluid communication with therespective well 14.

[0083] As best seen in FIGS. 17a, 17 b, the flow-through manifold 600 issubstantially identical to the general use manifold assembly 56, andthus can include an elongated stainless steel manifold bar 55. Themanifold bar 55 can include a plurality of inlet/outlet port pairs 602,602′, wherein the inlet/outlet ports 602, 602′ are formed in themanifold bar 55 using known machining techniques. The inlet/outlet ports602, 602′ are each surrounded by an O-ring interface 53 a′, 53 b′.

[0084] As best seen in FIGS. 17a, b, the flow-through manifold 600differs from the general use manifold 56 in that each inlet/outlet port602 can be joined in fluid communication so as to create a common flowpath 604 through the manifold bar 55, while each inlet/outlet port 602′defines separate flow paths 606 through the manifold bar 55 as best seenin FIG. 17a.

[0085] When a single flow-through manifold bar 55 is coupled to thereactor block 12 at sidewall surface 22 b, each inlet/outlet port 602aligns with a single opening 20 so as to establish a common fluid flowpath 604 between each inlet/outlet port 602 and each flow path 20 a. Andeach inlet/outlet port 602′ aligns with separate openings 21,establishing fluid communication with the associated flow path 21 a.

[0086] If a second flow-through manifold bar 55 is coupled to sidewallsurface 22 b′, each inlet/outlet port 602 aligns with a single opening20 so as to establish a common fluid flow path 604 between eachinlet/outlet port 602 and each flow path 20 b. And each inlet/outletport 602′ aligns with a separate opening 21, establishing fluidcommunication with the associated flow path 21 b.

[0087] The flow-through manifold 600 allows one fluid supply, preferablya gas supply, to feed all eight reactor wells 14 via the associated flowpath 20 a or 20 b. This arrangement requires fewer hoses or connectorsthan the general use manifold 56 to establish fluid communicationbetween the manifold inlet/outlet ports 602, 602′ and flow paths 20 a,20 b. This arrangement also permits each flow path 21 a, 21 b to bevented separately to the head space 17 as previously discussed, and outof the reactor block 12 to ambient conditions, if necessary. Further,the respective flow paths 21 a, 21 b can be plugged using knowntechniques if venting to the head space 17 is not necessary orundesirable.

[0088] Alternatively, the inlet/outlet ports 602, 602′ can be configuredso as to define separate flow paths through the manifold bar 55. Thisarrangement can be used where it is desirable to have different gas flowrequirements for each well 14, and results in a setup identical to thatof the general use manifold 56.

[0089] Static Pressure Manifold

[0090] In still another embodiment, the general use manifold assembly 56can be configured as a static pressure manifold 700, as best seen inFIGS. 18a, b. It will be appreciated that the general use manifoldassembly 56 and the static pressure manifold 700 share common elements.Thus, common reference numerals are used to describe common features.The static pressure manifold 700 is virtually identical to the generalmanifold assembly 56, and includes a metal manifold bar 55 defining aplurality of inlet/outlet port pairs 702, 702′. The inlet/outlet ports702, 702′ are each separately surrounded by an O-ring interface 53 a′,53 b′.

[0091] The static pressure manifold 700 differs from the general usemanifold assembly 56 in that each inlet/outlet port 702 is joined influid communication, as best seen in FIG. 18b. This arrangement permitsa common flow path 704 through the eight inlet/outlets 702, as best seenin FIG. 18a. However, each of the eight inlet/outlet port 702′ candefine separate flow paths 706 through the manifold bar 55.

[0092] When a single static pressure manifold bar 55 is coupled to thereactor block 12 at sidewall surface 22 b, each inlet/outlet port 702aligns with an opening 21 so as to establish fluid communication withand a common flow-through each respective flow path 21 a, and eachinlet/outlet port 702′ aligns with an opening 20 to establish fluidcommunication with a respective flow path 20 a. This arrangement allowsone gas supply to feed all eight reactor wells 14 via the flow path 21a, thus simplifying the assembly in comparison to the general manifold56. This arrangement also permits the establishment of a common pressureat each reactor well 14 via each flow path 21 a. If a second staticpressure manifold bar 55 is coupled to the sidewall surface 22 b′, eachinlet/outlet port 702 aligns with an opening 21 so as to establish fluidcommunication with and a common flow-through each flow path 21 b, andeach inlet/outlet port 702′ aligns with an opening 20 to establish fluidcommunication with a respective flow path 20 b.

[0093] Using the described arrangement of two static pressure manifoldbars 55 coupled to opposing sides of the reactor block 12, each flowpath 21 a is joined to a common pressure source and each flow path 21 bis vented through a common flow path. Yet the flow paths 20 a, 20 b canbe separately coupled to fluid sources or vented or plugged as desired.

[0094] The static pressure manifold 700, like the flow-through manifold600, can permit a fluid, preferably a gas, or additional chemistry to beadded to or a sample to be withdrawn from each vessel 16 or well 14 viathe respective flow path 21 a, 21 b. And if a particular flow path 20 a,20 b (also applies to flow paths 21 a, 21 b) is not needed for aparticular experiment, the respective flow path or the inlet thereto canbe plugged using known techniques. And under certain conditions one ofthe flow paths 21 a or 21 b can be vented to the head space 17 while theother flow path 21 a or 21 b is coupled to a single fluid source.

[0095] In an alternative embodiment, each inlet/outlet port 702 can beconfigured so as to define separate flow paths through the manifold bar55. This configuration would result in an assembly identical to that ofthe general use manifold 56.

[0096] Each of the manifold assemblies 56, 600 and 700 can be usedinterchangeably. That is, a single general use manifold 56, flow-throughmanifold 600 or a static pressure manifold 700 could be used inconjunction with another general use manifold 56, flow-through manifold600, or a static pressure manifold 700. The interchangeability of thevarious manifolds 56, 600 and 700 permits the user to establish avariety of flow paths through the reactor block 12.

[0097] Stir Top Assembly

[0098] One function of the stir top assembly 26 is to permit agitationof the reaction mixtures during the experiment. FIGS. 6-10 show a stirtop assembly 26 formed in accordance with the teachings of thisinvention, and, more particularly, FIGS. 8 and 9 show a perspective viewof the stir top assembly 26 formed in accordance with the teachings ofthis invention.

[0099] As best seen in FIGS. 8 and 9, the stir top assembly 26 caninclude an injector plate 28 having a top surface 28 a, bottom surface28 b and a sidewall surface 28 c, a stirring blade assembly 30, one ormore dip tubes 32 a, 32 b and a cover 31 a.

[0100] Injector Plate

[0101] As shown in FIG. 9, the injector plate 28 defines a plurality ofopenings for supporting various components. As best seen in FIG. 9, thebottom surface 28 b of the injector plate 28 defines one or more holes(not shown) for receiving a dowel pin 24. As shown in FIG. 9, two dowelpins 24 are supported by the injector plate 28. The dowel pins 24provide a means for aligning the stir top assembly 26 with the reactorblock 12, as best seen in FIG. 2a. The dowel pins 24 can include asmooth outer perimeter that frictionally engages the outer perimeter ofthe mating opening, or the dowel pins 24 can include a threaded surfacethat mates with threads supported by the mating hole.

[0102] As best seen in FIG. 9, the injector block 28 defines one or moremounting holes 25 a for receiving threaded fasteners such as screws forcoupling the injector plate 28 to the cover 31 a (discussed in moredetail below). The injector plate 28 can also include a plurality ofopenings 25 b along the length of its sidewall 28 c, as best seen inFIG. 9. The openings 25 b receive threaded fasteners such as bolts orscrews for coupling the injector plate 28 to the manifold assembly 56,600 or 700.

[0103] As best seen in FIGS. 2b, 8 and 9, the injector plate 28 can alsoinclude a plurality of openings 65 for receiving threaded fasteners forcoupling the injector plate 28 to an adjacent component. The injectorplate 28, as shown in FIG. 9, can include an opening 34 b for receivinga shaft 36 for coupling the motor 19 to the stir top assembly 26.

[0104] As shown in FIG. 9, the injector plate 28 can also include aplurality of openings 51. As best seen in FIG. 5, a delivery tube 37 ais received in and extends downwardly from each opening 51. Eachdelivery tube 37 a allows the injection of chemistry into one or morewells 14. As best seen in FIG. 5, each delivery tube 37 a extends into asingle reactor well 14. Preferably, the delivery tube 37 a extends belowthe surface of the sample contained in the respective reactor well 14 asshown in FIG. 5. The delivery tube 37 a can be fabricated of a polymersuch as glass or plastic or any other material that is chemically inertto the sample and/or the fluid being injected into the well 14.

[0105] Also, as shown in FIG. 5, the injector plate 28 defines a flowpath 37 b. The flow path 37 b is in fluid communication with thedelivery tube 37 a, and extends laterally through the injector plate 28,terminating at the injector plate sidewall surface 28 c.

[0106] Referring back to FIG. 9, the injector plate 28 also includes aplurality of openings 41. As best seen in FIG. 7, the openings 41 canreceive a collar 44, such as a threaded insert, sleeve or nut, by aninterference fit for supporting a mating component.

[0107] As shown in FIGS. 9 and 7, the injector plate 28 also defines aplurality of fluid openings 33. As best seen in FIG. 7, each opening 33is in fluid communication with respective flow paths 33 a, 33 b. As bestseen in FIGS. 5 and 7, each flow path 33 a, 33 b extends angularlyupwards through the injector plate 28 and terminates at respectiveinternal openings 35 a, 35 b defined by an interior portion of theinjector plate 28.

[0108] The injection plate 28 can be formed of a metal, preferablystainless steel. It will be appreciated that all openings and flow pathsformed therein can be formed using known machining or metal workingtechniques.

[0109] Stirring Blade Assembly

[0110] As shown in FIG. 9, the injector plate 28 can further include aplurality of mounting holes 59 for supporting the stirring bladeassembly 30 (discussed in more detail below). As best seen in FIGS. 6and 9, the stirring blade assembly 30 comprises a plurality of stirringmembers, preferably one stirring member for each well 14, and includes aspindle 38 and a stirring blade 40. The stirring blade assembly 30 ofthe present invention is identical to that described in U.S. applicationSer. No. 09/548,848, the discussion of which is incorporated herein byreference.

[0111] Turning first to the stirring blade 40, as shown in FIGS. 6 and8, the stirring blade 40 can be configured as a substantially planarhooked-shaped finger. The finger can be fabricated of a polymer such asglass or plastic or a coated metal, provided the selected material doesnot react with the chemistry in the vessel 16 (or well 14). It will beunderstood that the stirring blade 40 can be configured using a varietyof simple or complex geometric configurations, including but not limitedto rectangular, circular, etc.

[0112] As best seen in FIGS. 6 and 7, the spindle 38 can be an elongatedmetal bar, with the preferred metal being stainless steel. The spindle38 can include a first end 38 a and a second end 38 b, the first end 38a being rotatably coupled to the stirring blade 40 using knowntechniques.

[0113] The second end 38 b of the spindle 38 is mechanically coupled toa gear 43 in accordance with conventional mounting techniques, as bestseen in FIG. 7. The gear 43 is supported by the second end 38 b of thespindle 38 such that the gear 43 meshes with an adjacent gear 43, asbest seen in FIG. 6. The combination of adjacent meshed gears 43 forms agear train that is accessible through the cover 31 a for driving thespindle 38 and the associated stirring blade 40. The gears 43 formingthe gear train can be conventional gears of the type generally used forforming a direct drive gear train assembly, wherein the gear traindirectly drives one or more components coupled to each individual gearof the gear train.

[0114] The gear train (the plurality of meshed gears 43) is coupled to amagnetic feed through 42 using known techniques. The magnetic feedthrough 42 couples the gear train to the first end 38 a of the spindle38, as best seen in FIG. 6. The spindle 38 mechanically couples themotor 19 to the gear train such that the rotational speed of the motor19 is proportional or identical to the torque applied to the spindle 38and the stirring blade 40.

[0115] The motor 19 provides sufficient torque for rotating the stirringblades 40 at the same speed. For instance, the stirring blade 40 can berotated at a speed varying from approximately zero to 3,000 rpm, andeven more particularly from approximately 100 rpm to approximately 1,000rpm. The rotational speed of the motor 19 can be monitored via a motorspeed controller 132 (discussed in detail in the subsection describingthe heater and motor control box 116)

[0116] It will be appreciated that alternative drive means such as, butnot limited to, belts, chains or sprockets, a combination of theaforementioned, magnetic followers or other drive mechanisms could beused to power the stirring blade assembly 30.

Dip Tubes

[0117] As best seen in FIGS. 5, 6 and 7, the reactor block assembly 12supports a plurality of dip tube pairs 32 a, 32 b, preferably one diptube 32 a, 32 b pair for each well 14. The dip tubes 32 a, 32 b cancomprise hollow open-ended tubular members having a first end 39 a and asecond end 39 b. Each dip tube 32 a, 32 b can be made of glass, plastic,coated metal tubes or any material that will not chemically react withthe reaction mixtures.

[0118] Each dip tube 32 a, 32 b is positioned within a mounting hole 51such that the stirring blade assembly 30 is positioned intermediate thedip tubes 32 a, 32 b as best seen in FIGS. 5, 6 and 7. Specifically, thefirst end 39 a of each dip tube 32 a, 32 b is supported by the collar44, the collar 44 being sized to frictionally engage a portion of theperimeter of each dip tube 32 a, 32 b to secure each dip tube 32 a, 32 bin position. As best seen in FIGS. 5 and 7, each dip tube pair 32 a, 32b extends downwardly from the respective mounting holes 51 in parallelrelationship. Additionally, as best seen in FIG. 6, a filter 45 issupported by the top surface of the collar 44 above each dip tube 32 a,32 b to permit filtering of the sample, if any, withdrawn from thereactor well 14 or fluids injected into the reactor well via the diptubes 32 a, 32.

Cover

[0119] As best seen in FIG. 9, the top surface 28 a of the injectorplate 28 is partially enclosed by a cover 31 a so as to enclose the geardrive assembly 43 supported by the injector plate 28. The cover 31 a canbe secured to the injector plate 28 by screws (not shown) inserted intomating openings defined by the cover 31 a and the bottom surface 28 b ofthe injector plate 28.

[0120] As best seen in FIG. 8, the cover 31 a is a substantiallyelongated member and defines a plurality of indentations 31 b. As shownin FIG. 8, the cover 31 a can include eight indentations 31 b. Eachindentation 31 b defines a gripping surface that helps facilitate handcarrying the reactor block 12.

[0121] As shown in FIG. 8, the cover 31 a also includes an opening 34 a.The opening 34 a can be formed using known machining techniques. As bestin FIGS. 4 and 8, the opening 34 a receives a shaft 36, the shaft 36having a first end and a second end, wherein the first end supports ascrew cap 34. The second end engages a slot 146 defined by the motor 19shaft, as best seen in FIG. 4.

[0122] The cover 31 a is preferably fabricated of aluminum using knownmachining or metal working techniques. And it will be appreciated thatother materials having similar chemical, thermal or material propertiescould be used.

Stir Top Injection Manifold Assembly

[0123] Referring back to FIGS. 8 and 9, if desirable, the stir topassembly 26 can support an injection manifold 46, which allowsadditional chemistry such as catalysts, solutions, slurries or othercomponents to be added to one or more vessels 16 (or each reactor well14 if no vessel 16 is used) during an experiment. The injection can takeplace under pressure and without reducing the pressure in the vessels 16or wells 14. The injection manifold 46 can include a standard metalmanifold bar 47, with the preferred metal being stainless steel.

[0124] As best seen in FIG. 8, the manifold bar 47 can include a firstplurality of openings 29 for receiving threaded fasteners for couplingthe manifold bar 47 to the injector plate 28. The manifold bar 47 alsodefines a second plurality of axially aligned openings 49, wherein theopenings 49 are added to reduce the weight of the manifold bar 47.

[0125] As best seen in FIG. 8, the manifold bar 47 also defines a secondplurality of openings 50 for receiving a threaded fill port cap 52. Thefill port cap 52 includes an elongated body 52′ having a longitudinalaxis and a bore 68 centered on the longitudinal axis. The bore 68 canextend the length of the elongated body 52′, and can receive and supporta cylindrical sleeve or fitting 74 having a through hole centered on theaxis of the fitting 74. The fitting 74 can be fabricated of a chemicallyresistant plastic such as perfluro-elastomer or polyethyethylketone orpolytetrafluoroethylene. As best seen in FIGS. 5 and 8, the fitting 74can be seated within the bore 68 of the elongated body 52′, and cansupport at least one injector or delivery probe 48 by an interferencefit with an O-ring seal (not shown) or other similar sealing device. Theinjector or delivery probe 48 can be a hollow glass, plastic or coatedmetal open-ended tube.

[0126] One or more conduits or vessels (not shown) can be used to couplethe delivery probe 48 to components to be injected into the vessel 16.Alternatively, the delivery probe 48 or the bore 68 could be placed indirect fluid communication with a delivery device such as a syringe orother similar device for injecting the chemistry or other componentsinto one or more vessels 16. It will be appreciated that the same ordifferent chemistry or other components can be injected into the one ormore vessels 16 using the injection manifold 46.

[0127] Referring back to FIGS. 5 and 6, the fill port cap 52 alsosupports a plug 52 a for opening and closing a flow path 50 a machinedthrough the manifold bar 47 wherein separate flow path 50 a are in fluidcommunication with each respective well 14. As best seen in FIG. 5, eachflow path 50 a extends through a portion of the sidewall surface of theinjection manifold bar 47, and is in fluid communication with flow path37 b of the stir top assembly 26. Thus, the flow path 50 a couples theinjection manifold 46 in fluid communication with the reactor block 12via the flow path 37 b and associated delivery tube 37 a.

[0128] As best seen in FIG. 6 when the fill port cap 52 is tighteneddown, the plug 52 a blocks fluid flow-through the respective flow path50 a, and consequently flow to the delivery tube 37 a and the associatedflow path 37 b. When the screw cap 52 is loosened and backed slightlyout of the opening 50, the plug 52 a is backed out of the flow path 50a, thus allowing fluid flow-through the respective flow path 50 a and,consequently, through the flow path 37 b and associated delivery tube 37a.

[0129] In an alternative embodiment, the stir top assembly 26 cansupport a blank manifold 54, as best seen in FIG. 10. The blank manifold54, like the injection manifold 46, can include an elongated stainlesssteel bar 47. The blank manifold 54 can define a plurality of axiallyaligned threaded holes 54 a for receiving threaded fasteners such asscrews or bolts for plugging the flow path 37 b through the injectorplate 28.

[0130] Regardless of the embodiment of the manifold configuration 46 or54 used, either manifold assembly 46, 54 can be coupled to the injectorplate 28 via threaded fasteners. As best seen in FIG. 10, the manifold46 or the blank manifold 54 can be attached to the injector plate byinserting threaded fasteners into aligned openings 54 a and 25 b definedby the injection manifold 46 and the injector plate 28, respectively. Ifthe injection manifold 46 is used instead, the threaded fasteners areinserted through aligned openings 29 and 25 b, wherein opening 29 isdefined by the injection manifold bar 47.

[0131] Sampling Manifold Assembly

[0132] Turning now to FIGS. 12-15, a sampling manifold assembly 58 isshown formed in accordance with the teachings of the present invention.The sampling manifold assembly 58 allows the removal of a small volumeof the reaction mixture from a pressurized vessel 16 (or vessel 14)during or after an experiment. As best seen in FIGS. 12, 13, thesampling manifold 58 can include a manifold plate 60, a plurality offlow control valves 62, 64, and 66, and a sample vial 98.

[0133] The manifold plate 60 can be a planar rectangular metal plateformed using known metal working techniques. One of skill in the artwill appreciate that the manifold plate 60 can be formed using othersimple or complex geometric configurations, including, but not limitedto circular, hexagonal, triangular, etc. In the disclosed embodiment,the manifold plate 60 defines a plurality of openings (not shown) forreceiving and supporting the flow control valves 62, 64, 66 as best seenin FIGS. 12, 13. The holes can be formed in the plate 60 using knowmachining or metal working techniques.

[0134] Turning now to a more detailed discussion of each flow controlvalve 62, 64, and 66, the first flow control valve 62 can be a standard2-way needle valve of the type typically used in the industry, as bestillustrated in FIG. 15. The first flow control valve 62 can include avalve body 70 a and a rotatable control knob 70 b, as best seen in FIGS.13, 14. As best seen in FIG. 15, the control knob 70 b opens and closesa fluid flow path 80 through the flow control valve 62.

[0135] The first flow control valve 62 can also include an inlet port 76and an outlet port 82. The inlet port 76 is opened and closed byrotating the rotatable knob 70 b, wherein the knob 70 b can beselectively rotated so as to expose the inlet port 76 to ambientconditions (open position) or rotated so as to seal the inlet port 76,isolating the inlet port 76 from ambient conditions (closed position)and closing flow path 80.

[0136] As shown in FIGS. 13, 14, the inlet port 76 supports a firststainless steel hollow, open-ended tubular member 72 via a standardfitting, wherein one end of the first tubular member 72 is in fluidcommunication with a vessel 16 (or well 14) via a respective dip tube 32a, 32 b. The outlet port 82 is formed on the valve 62 at approximately90° below the inlet port 76. The outlet port 82 supports a secondstainless steel hollow, open-ended tubular member 83 of the typepreviously described. The second tubular member 83 is also supported inthe outlet port 82 via a standard fitting.

[0137] The second flow control valve 64 can be a standard normally openvalve, as best illustrated in FIG. 15. As shown in FIGS. 13, 14, thesecond flow control valve 64 can include a valve body 90 a and arotatable control knob 90 b, wherein the control knob 90 b can berotated to establish fluid communication between a fluid flow path 85through the flow control valve 64 and a sample vial 98 (discussed inmore detail below), as best seen in FIG. 15.

[0138] As shown in FIG. 13, the second flow control valve 64 includesfirst and second inlet/outlet ports 84, 86 and an outlet port 88. Theinlet port 84 is defined at a first position 92 on the flow controlvalve 64, wherein the first position 92 is located on the valve 64 bodyat approximately 90° above the rotatable knob 90 b. The inlet port 84receives the opposite end of the second tubular member 83 supported bythe first flow control valve 62.

[0139] As also shown in FIG. 13, the second inlet/outlet port 86 isformed on the valve body 90 a at a location approximately 180° below thefirst position 92 and approximately 90° below the control knob 90 b. Thesecond inlet/outlet port 86 supports a third hollow tubular member 94 ofthe type previously described.

[0140] As shown in FIG. 13, the inlet/outlet port 88 is located on thevalve 64 body at a position approximately 180° relative to the positionof the control knob 90 b or 90° to the left of the first position 92.The outlet port 88 supports a fourth hollow tubular member 96 of thetype previously described. As shown in FIG. 13, the opposite end of thehollow fourth tubular member 96 is in fluid communication with thesample vial 98 (discussed in more detail below).

[0141] As best seen in FIG. 15, the third flow control valve 66 can be aconventional 2-way needle valve. As shown in FIGS. 13, 14, the thirdflow control valve 66 includes a body 102 a and a rotatable control knob102 b, wherein the rotatable control knob 102 b open and closes a flowpath 104 through the valve body 102 a, as best seen in FIG. 15.

[0142] As shown in FIG. 13, the valve 66 also includes an inlet port 106and an outlet port 108. The inlet port 106 is located on the valve body102 a at a position approximately 180° from the position of the controlknob 102 b. The inlet port 106 supports one end of a fifth hollowtubular member 110 of the type previously described via a standardfitting. The opposite end of the fifth tubular member 110 is coupled toa source of fluid under pressure 112 also via an interference fit.

[0143] The source of fluid under pressure can be a low pressure nitrogengas or other gas or fluid that will not react with the sample fluid, thevalves or tubing with which the pressurized fluid comes into contact.The outlet port 108 is located on the valve body 102 b approximately 90°above the position of the control knob 102 b, and is in fluidcommunication with the second valve 64 via the third tubular member 94.

[0144] As shown in FIG. 14, the valves 62, 64, and 66 can be alignedalong the manifold plate 60 such that the first flow control valve 62 ispositioned at the upper portion of the manifold plate 60, the secondflow control valve 64 is positioned at a lower position on the manifoldplate 60, and the third flow control valve 66 is positioned below thesecond valve 64 such that the second flow control valve 64 is positionedintermediate the valves 62 and 66.

[0145] As best seen in FIGS. 13, 14, eight flow control valves 62, 64,66, respectively, are coupled to the manifold plate so as to form asingle row R1, R2, R3, wherein the respective rows includes eight valves62, 64 or 66. As best seen in FIGS. 13, 14, row R1 includes only flowcontrol valves 62, row R2 includes only flow control valves 64, and rowR3 includes only flow control valves 66. Each adjacent control valve 62,64 and 66, respectively, is separated by a spacer 69, as best seen inFIG. 13. Each valve 62, 64, and 66 is mounted onto the manifold plate 60such that the valve body 70 a, 90 a, 102 a, respectively, protrudes fromthe rear of the manifold plate and the rotatable knob 70 b, 90 b, 102 b,respectively, protrudes from the front of the manifold plate 60.

[0146] As best seen in FIG. 14, each row R1, R2, R3 of valves 62, 64,66, respectively, is coupled to the manifold plate 60 via a mountingbracket 71. The mounting bracket 71 includes a first portion and asecond portion 71 a, 71 b defining a pair of openings 73 of the mountingbracket 71. Each opening 73 aligns with openings (not shown) defined byeach valve 62, 64 and 66.

[0147] As shown in FIG. 14, a rod 78, preferably threaded, is insertedthrough the respective openings defined by the valves 62, 64, and 66 andthe respective mating openings 73. The rod 78 extends through each ofthe respective valves 62, 64, and 66 forming the respective row ofvalves R1, R2, and R3. One end 79 of the rod 78 supports a nut or otherthreaded sleeve (not shown) for coupling the rod to the mounting bracketfirst portion 71 a, and the mounting bracket first portion 71 a iscoupled to the manifold plate 60 via the mounting bracket second portion71 b. The mounting bracket second portion 71 b, as best seen in FIG. 14,can be attached to the manifold plate 60 by inserting threaded fastenerssuch as screws or other similar devices through the openings 73.

[0148] Now referring back to FIG. 12, the sample vial 98 can comprise anenclosed cylindrical container 113. The cylindrical container 113 caninclude a first surface 114 defining an open top 115 for receiving oneend of the fourth tubular member 96.

[0149] Heater and Motor Control Box

[0150] The heater and motor control box 116 permits separate control ofthe temperature of each reactor well 14. As best seen in FIG. 11, thereis one heater controller 120 for each reactor well 14, and a singlemotor control 122 for controlling the motor 19. As shown in FIGS. 1 and11, the heater and motor control box 116 of the present invention caninclude a base 118; a temperature control system 117 including heatercontrollers 120, microprocessors 123, temperature display devices 124,and a solid state relay 128; and a motor controller 122.

[0151] As shown in FIGS. 1 and 11, the base 118 retains the componentscomprising the heater and motor control box 116, and includes aremovable top surface 119 and sidewall surfaces 125, 127. The topsurface 119 can define a plurality of mounting holes 121 for receivingthreaded fasteners such as screws for coupling the top surface 119 tothe sidewalls 125, 127. The top surface 119 can also include a pluralityof vent holes 126 to allow air circulation thorough the heater and motorcontrol box 116.

[0152] Each sidewall surface 125, 127 defines one or more openingsformed therein using known machining or metal working techniques. Thesidewall surfaces 125 define a plurality of openings 129 for couplingthe sidewall 125 to the an adjacent sidewall surface. The sidewall 125also defines a vent opening 126 which cooperates with the vent 126defined in the top surface 119 to permit air circulation through theheater and motor control box 116.

[0153] Sidewall surface 127 defines a plurality of openings (not shown)for supporting electrical connectors or interface plugs 136 using knownmounting techniques. The connectors or interface plugs 136 can besupported in the openings (not shown) using an interference fit.Additionally, the electrical connectors 136 can be of a type generallyknown and used in the industry, and electrical wiring to be coupledthereto can be attached to the electrical connectors or interface plugs136 in accordance with known wiring techniques.

[0154] As shown in FIG. 11, the sidewall surface 127 also defines aplurality of openings (not shown) for receiving and supporting a motoron/off switch 135 for controlling the operation of the motor 19. Thesidewall surface 127 also supports a motor speed control 132, whichpermits adjustment of the speed of the motor 19. Also shown in FIG. 11,the sidewall surface 127 supports a display panel for the motor speedcontrol 134. The display screen 134 can include a standard displaydevice such as a liquid crystal display or other similar device thatdisplays digital or analog information indicative of the speed of motor19.

[0155] The sidewall surface 127 also supports a display screen 124 forthe heater controller 120. The display screen 124 can include a standarddisplay device such as a liquid crystal display or other similar devicefor displaying digital or analog information indicative of, or that canbe used to determine, the temperature of the reactor well 14 inelectrical communication with the display screen 124. As shown in FIG.1, the display screen 124 can support a selectively adjustabletemperature control switch 142. The temperature control switch 142permits a user to manually increase or decrease the desired temperatureof the respective reactor well 14, vessel 16 or both.

[0156] In addition to the display screen 124, each heater controller 120can also include a microprocessor 123 for monitoring and adjustment ofthe temperature of the heating device 99. It will be appreciated thatthe microprocessor 123 is electrically coupled to the temperaturecontrol switch 142, permitting user variation of the desired temperatureof the reactor well 14, vessel 16 or both.

[0157] To control the supply of power to the heating devices 100, themicroprocessor 123 can be electrically coupled to a conventional solidstate relay 128, as shown in FIG. 11. The solid state relay 128 can becaused to become active by depressing the temperature control switch142, i.e., to increase or decrease the power to the heating device 99.In the disclosed embodiment, the solid state relay 128 can be activatedby activating the control switch 142 supported by the display screen124.

[0158] To aid the temperature sensing function of the microprocessor123, the microprocessor 123 can be electrically coupled to a temperaturesensor 144 such as a thermocouple. As best seen in FIG. 2a, thetemperature sensor 144 can be inserted into channel 133 defined by thewell body 14 a. This arrangement establishes thermal contact between thetemperature sensor 144 and the respective reactor well 14. When themicroprocessor 123 via the temperature sensor 144 detects a temperatureabove or below the selected temperature, the microprocessor 123 cancause the activation of the solid state relay 128

[0159] In operation, heating of the reactor wells 14 or vessels 16, orboth can occur by electrically coupling the microprocessor 123 to aheating device 99 for each respective well 14 and placing the heatingdevice 99 in thermal contact with a respective well 14, as shown inFIGS. 2a and 3 d. The heating device 99 can be a pair of heating probesthat can be inserted into the respective well 14 through channels 130formed along the perimeter of each well 14, as best seen in FIG. 2a and3 d. Each heating device 99 can be placed in thermal contact with thetemperature sensor 144, wherein the temperature sensor 144 iselectrically coupled to the microprocessor 123.

[0160] The microprocessor 123 is electrically coupled to the displayscreen 124 such that the display screen 124 displays informationindicative of the temperature (or information that can be used tocalculate the temperature) of the particular heating device 99, reactorwell 14 or vessel 16.

[0161] Depending on the application, each reactor well 14 or vessel 16can be maintained at the same temperature or at different temperaturesduring an experiment. For example, one may screen compounds forcatalytic activity by first combining, in separate vessels 16, each ofthe compounds with common starting materials; these mixtures can beallowed to react at uniform temperature. One may then furthercharacterize a promising catalyst by combining it in numerous vesselswith the same starting materials used in the screening step. Themixtures can be allowed to react at different temperatures to gauge theinfluence of temperature on catalyst performance (speed, selectivity).

[0162] Referring back to FIG. 11b, the motor controller 122 is of a typeknown in the industry, and is secured to the base 118 using threadedfasteners such as screws. The motor controller 122 is electricallycoupled to the motor 19 using conventional wiring techniques. The motorcontroller 122 can also be electrically coupled to a motor speed control132 to allow adjustment of the speed of the motor 19. As best seen inFIG. 11, the speed of the motor 19 can be monitored via a motor speedreadout 134 supported by the base 118 via an interference fit. The motorspeed readout 134 displays digital or analog data indicative of themotor 19 speed or information that can be used to compute motor 19speed.

[0163] The motor controller 122 described herein is manually adjustable.However, the motor controller 122 could be adjusted automatically via acomputer or microprocessor as described in U.S. application Ser. No.09/548,848, the discussion of which is incorporated herein by reference.

Assembly

[0164] The parallel reactor 10 can be easily assembled by assemblingtogether the various subsystems, e.g., the reactor block 12, the stirtop assembly 26, the manifold assembly 56, the sampling manifoldassembly 58, and the heater and motor control box 116. The subassembliescan be assembled together as follows to form the parallel reactor 10:

[0165] As best seen in FIG. 2a, the reactor block 12 can be assembled inthe manner previously described wherein the legs 18 are attached to thereactor block 12 using threaded fasteners. As shown in FIG. 1, thereactor block 12 can be supported by the heater and motor control box116 by inserting threaded fasteners into openings 138 defined by foot 18d of leg 18 and mating openings (not show) defined by the top surface119 of the heat and motor control box 116.

[0166] As shown in FIG. 2a, the stir top assembly 26, having beenassembled in the manner described herein, can be coupled to the reactorblock 12 such that the surface 28 b of the injector plate 28 seals thereactor wells 14 from ambient conditions. The stir top assembly 26 iscoupled to the reactor block 12 by aligning the dowel pin 24 with matingopenings 11 b formed in the reactor block 12. Prior to inserting thedowel pin 24 into the mating opening 11 b, O-ring seals can be placed inthe respective O-ring interfaces 13 and 27, as best seen in FIGS. 3a, 3b. The dowel pin 24 can then be inserted into the mating opening 11 b,and threaded fasteners such as screws or bolts can be passed thoughcentrally aligned openings 11 a, 65 defined by the injector plate 28 andthe top surface 22 a of the reactor block 12 a, respectively. Referringnow to FIG. 7, when the reactor block 12 and the stir top assembly 26are assembled, the respective openings 27 formed in the top surface 22 aof the reactor block 12 a align with a respective opening 33 defined bythe injector plate 28 of the stir top assembly 26.

[0167] Additionally, when the stir top assembly 26 is in place, thestirring blade assembly 30 extends into the vessel 16 such that aportion of the stirring blade 40 lightly contacts the bottom of vessel16, as best shown in FIG. 6. In another embodiment, the stirring blade40 could be suspended just above, but not in contact with, the bottom ofthe vessel 16, as best seen in FIG. 5.

[0168] Also, as shown in FIG. 2a, the shaft 36 is coupled to the motorshaft 19 a. The threaded knob 34 supported by one end of the shaft 36 istightened down such that the shaft 36 engages a slot 146 defined by themotor shaft 19 a. This arrangement couples the motor 19 to the shaft 36by an interference fit.

[0169] The sampling manifold 58 can be coupled to the reactor block 12via the manifold assembly 56, flow-through manifold 600 or the staticpressure manifold 700. Regardless of the manifold assembly used 56, 600or 700, the first tubular member 72 supported by each first flow controlvalve 62 is received in a respective manifold inlet/outlet opening 53 a,53 b so as to couple the respective control valve 62 in fluidcommunication with a respective flow path 20 a, 20 b, as best seen inFIG. 1. As shown in FIG. 1, the inlet port 76 of a respective flowcontrol valve 62 is coupled to a respective opening 20 via therespective hollow tubular member 72 by a standard fitting. The outletport 82 of the respective first flow control valve 62 is coupled influid communication with the input port 84 of the respective verticallyadjacent flow control valve 64 also using an interference fit, and therespective output port 86 of the respective second flow control valve 64is coupled in fluid communication with the respective inlet/outlet port108 of the respective third flow control valve 66 via a respectivefourth tubular member 94.

[0170] Alternatively, the sampling manifold 58 can be coupled directlyto the reactor block 12 as best seen in FIG. 20. In this arrangement,the first tubular members 72 are coupled in fluid communication with therespective flow paths 20 a, 20 b by an interference fit with an O-ringseal or other similar sealing device.

[0171] As an alternative embodiment, the parallel reactor 10 could beplaced in a chamber 100, as shown in FIG. 1. The chamber 100 can beevacuated or filled with a desirable gas, such as an inert gas likenitrogen or argon. Alternatively, the chamber could be filled with gasfor charging or inducing a pressure at each reactor well 14. In othercases, the chamber 100 may be used only during the loading of startingmaterials into the wells 14 to minimize contamination during samplepreparation, for example, to prevent contamination of oxygen sensitivecatalysts. The chamber 100 is most usefully a glove box (or dry box),such as those sold commercially by Vacuum Atmospheres, Inc.

Operation

[0172] Up to eight different reaction mixtures can be processed during asingle experiment conducted using the parallel reactor 10. Thus, not allreactor wells 14 must be used during a single experiment. And the sameor different reaction mixtures can be added to the selected vessels 16.The reaction mixtures can be manually added to the selected vessels 16.Alternatively, a robotic material handling system 200 could be used toload the reaction mixtures into each of the vessels 16, as illustratedin FIG. 19.

[0173] The robotic system 200 is of a type known in the industry, andincludes a pipette or probe 202 that dispenses measured amounts ofliquids into each of the vessels 16. The robotic system 200 manipulatesthe probe 202 using a 3-axis translation system 204. The probe 202 isconnected to sources 206 of chemistry or other reagents, preferably inliquid form, through flexible tubing 208. Pumps 210, which are locatedalong the flexible tubing 208, are used to transfer the chemistry fromthe sources 206 to the probe 202. Suitable pumps 210 include peristalticpumps and syringe pumps. A multi-port valve 212 located downstream ofthe pumps 210 selects which chemistry from the sources 206 is sent tothe probe 202 for dispensing in the vessels 16.

[0174] The robotic fluid handling system 200 is controlled by aprocessor 214. In the embodiment shown in FIG. 19, the user firstsupplies the processor 214 with operating parameters using a softwareinterface. Typical operating parameters include the coordinates of eachof the vessels 16 and the initial compositions of the reaction mixturesin individual vessels 16.

[0175] After addition of the chemistry to each well, the stir topassembly 26 is attached, and the reactor system 10 can be pressurized tostart the reaction process. The parallel reactor 10 is designed topermit experiments to be carried out at a maximum pressure ofapproximately 1500 psi and a maximum temperature of approximately 250°C. One of skill in the art will appreciate that the components of theparallel reactor 10 could be designed to accommodate a higher maximumpressure and temperature.

[0176] Heating the reaction mixtures, as well as temperature andpressure control, can play an important role in the reaction process.Heating and temperature are controlled by the heater and motor controlbox 116. Another important aspect of the present invention is theability to monitor and separately regulate the temperature of thereaction mixtures, as permitted by the heater and motor control box 116.

[0177] During synthesis, temperature can have a profound effect onstructure and properties of reaction mixtures. For example, in thesynthesis of organic molecules, yield and selectivity often dependstrongly on temperature. Similarly, in polymerization reactions, polymerstructure and properties, molecular weight, particle size, monomerconversion, and microstructure, can be influenced by reactiontemperature. During screening or characterization of combinatoriallibraries, temperature control and monitoring of library members isoften essential to making meaningful comparisons among members.

[0178] Temperature can also be used as a screening criteria or can beused to calculate useful process and product variables, includingmaterial properties. For instance, catalysts of exothermic reactions canbe ranked based on peak reaction temperature and/or total heat releasedover the course of reaction, and temperature measurements can be used tocompute rates of reaction and conversion.

[0179] Calorimetric Data Measurement and Use

[0180] Temperature measurements often provide a qualitative picture ofreaction kinetics and conversion and therefore can be used to screenlibrary members. For example, rates of change of temperature withrespect to time, as well as peak temperatures reached within each of thevessels 16 can be used to rank catalysts. Typically, the best catalystsof an exothermic reaction are those that, when combined with a set ofreaction mixtures, result in the greatest heat production in theshortest amount of time.

[0181] In addition to its use as a screening tool, temperaturemeasurements combined with proper thermal management and design of thereactor system can also be used to obtain quantitative calorimetricdata. From such data, scientists can, for example, compute instantaneousconversion and reaction rate, locate phase transitions (melting point,glass transition temperature) of reaction products, or measure latentheats to deduce structural information of polymeric materials, includingdegree of crystallinity and branching. U.S. application Ser. No.09/548,848 describes a system and method for obtaining calorimetric datameasurements, the discussion of which is hereby incorporated herein byreference.

[0182] Another important function of the present invention is theability to stir or agitate the reaction mixtures in situ by the stir topassembly 26. The stir top assembly 26 can be activated by causing themotor 19 to drive each of the stirring blade assemblies 30 at a uniformspeed. The stirring process can be continuous or repeated at selectedintervals throughout the experiment.

[0183] Mixing variables such as stirring blade torque, rotation rate,and geometry, may influence the course of a reaction and thereforeaffect the properties of the reaction products. For example, the overallheat transfer coefficient and the rate of viscous dissipation within thereaction mixture may depend on the stirring blade rate of rotation.Thus, in many instances it is important that one monitor and control therate of stirring of each reaction mixture to ensure uniform mixing,which in the disclosed embodiment is controlled by the motor speedcontroller 132.

[0184] Still another important aspect of the present invention is theability to add additional chemistry or other components to the reactionmixtures during the experiment without depressurizing the reactor wells14. The injection of materials into the vessel 16 can occur when thepressure of the vessel 16 is the same as or different from ambientpressure and at pressures ranging from ambient to approximately 1500psi.

[0185] The parallel reactor 10 permits fluids such as additionalchemistry to be introduced into, withdrawn from or vented through thereactor well 14. The introduction, withdrawal or venting of fluids cantake place at any point during or after the experiment without reducingthe pressure of the respective well 14. In the present invention theintroduction of fluids can occur via the injection manifold assembly 46or the reactor block manifold assemblies 56, 600 or 700.

[0186] Using the injection manifold 46, the introduction of one or morefluids or additional chemistry can be accomplished manually, by arobotic materials handling system as shown in FIG. 19 and using themethod previously described herein for using robotic materials handlingsystems or by other similar devices and techniques. The introduction,withdrawal or venting of fluids, including additional chemistry via thereactor block manifold assemblies will be illustrated with reference tothe flow-through manifold 600.

[0187] Conducting a Flow-Through Experiment Using the Flow-ThroughManifold

[0188] Referring back to FIG. 7, it may be desirable to introduce agaseous reactant, catalyst or other chemistry into the vessel 16. Usingthe flow-through manifold 600, each manifold inlet/outlet port 604 for asingle bar 602 is joined in fluid communication as previously describedand shown in FIGS. 17a and 17 b. The inlet ports 604 are coupled to acommon gas passage 608, and the common gas passage 608 is coupled to asingle gas source. Referring to FIG. 7, this assembly is then coupled,for example, to opening 20 so as to establish fluid communication withflow path 20 a, and the gas from the common gas source is injectedthrough common passage 608 into the inlet ports 604 and thus into theflow path 20 a where the gas is caused to be received in each associatevessel 16. Specifically, the gas travels through the flow path 20 a,through the flow path 33 a and into the opening 35 a where it isreceived in the dip tube 32 a and allowed to flow into the vessel 16.The introduction of the gas into the vessel 16 can occur even if thepressure of the vessel 16 is different from ambient conditions.

[0189] The introduction of the gas into the vessel 16 can cause apressure increase at the particular well 14. Thus, the well 14 can bevented to the head space 17 through flow path 21 b. To maintain theuniform gas flow rate through each respective well 14, the port to bevented to the head space 17 is generally opposite that through which thegas was introduced; hence the selection of flow path 21 b.

[0190] The remaining flow path can be coupled to the sampling manifold,for example the flow path 20 b would be coupled to the sampling manifold58 in the manner previously described, while the remaining flow paths 21a could be plugged or vented to the head space 17. This arrangementpermits a sample to be withdrawn from the vessel 16 through the flowpath 20 b using the procedure for withdrawing a sample previouslydiscussed.

[0191] If it is desirable to have different gas flow rates through theflow paths 20 a, each inlet port 604 of the flow-through manifold 600can be coupled to a separate gas supply.

[0192] Using the General Use Manifold 56 and Static Pressure Manifold700

[0193] The general use manifold 56 and the static pressure manifold 700can also be used in the manner previously described herein to providealternative flow paths and/or to permit the introduction of chemistryinto each vessel 16.

[0194] Withdrawing a Sample

[0195] Another important aspect of the parallel reactor 10 is theability to withdraw a sample from the reactor wells 14 at any timeduring the course of the experiment. The sample can be withdrawn whilethe well 14 is under pressure. Additionally the sample can be withdrawnwithout reducing the pressure in the well 14.

[0196] To withdraw a sample, the first tubular member 72 is coupled influid communication with the vessel 16; more particularly, the tubularmember 72 is coupled in fluid communication with the dip tube 32 a, asshown in FIG. 15. When the knob 70 b is rotated to open the first flowcontrol valve 62 to ambient conditions, the resultant pressure acrossdrop the tubular member 72 causes the back pressure in the well 14 topush a small volume of the sample out of the vessel 16 and into thesample loop 94 (third tubular member). More specifically, the path ofthe sample out of the respective vessel 16 could be as follows:

[0197] When the knob 70 b is rotated to the open position, a smallamount of the sample is pushed out of the vessel and into the dip tube32 a and exits the vessel 16 at the opening 35, as best illustrated bythe flow paths shown in FIG. 7. The sample continues through the flowpath 33 a and exits the stir top assembly 26 though the opening 33. Uponexiting the opening 33, the sample passes through the respective opening27 and enters the flow path 20 a and continues on through the opening20, where it enters the manifold assembly 56 inlet/outlet flow path 53 aand passes into first tubular member 72. The back pressure in the well14 (or vessel 16) causes the sample to continue through the tubularmember 72, through the valve 62, into the second tubular member 83 andthrough the normally open valve 64 to fill the sample loop (thirdtubular member 94).

[0198] Once the knob 70 b has been closed, the knob 90 b associated withthe second flow control valve 64 can be can be rotated so as to openflow path 85 between the second flow control valve 64 and the samplevial 98. Opening of the flow path 85, results in a pressure drop acrossthe sample loop 94 (third tubular member), thus causing the sample fluidto be pushed back through the second flow control valve 64 via the thirdtubular member 94, into the fourth tubular member 96 and finally intothe sample vial 98.

[0199] Once the sample has been deposited in the sample vial 98,residual amounts of the can sample remain in the tubular members 94, 96and the valve 64. These residual amounts of the sample can be flushedfrom tubular members 94, 96 by directing the nitrogen gas through thefifth tubular member 110 by rotating the control knob 102 b to open aflow path through the flow control valve 66 and the nitrogen gas.

[0200] When valve 66 has been opened, the nitrogen gas, preferably at apressure within the range of one and 20 psi, can be directed through thefifth tubular member 114. The low pressure gas flows through the valve66 and into the third tubular member 94, though the valve 64, andthrough the fourth tubular member 96, consequently forcing any residualamounts of the sample out of the tubular members 94, 96 and the valve62.

[0201] The parallel reactor 10 can be operated using semi-continuous orcontinuous processes, wherein chemistry can be metered into therespective wells 14 (vessels 16) at a controlled rate. Other processesare conducted in a continuous manner, where chemistry can be meteredinto the respective wells 14 (vessels 16) at a controlled rate, whileproducts or other chemistry is simultaneously removed from the reactor.

[0202] The flowing examples illustrate the principles and advantages ofthe invention.

EXAMPLE 1 Liquid Phase Hydrogenation Reaction (High Pressure Sampling)

[0203] The parallel reactor 10 can be used for chemical reactions suchas hydrogenation, oxidation, carbonylization and polymerization underpressure. The chemicals to be reacted can be in the form of a liquid,solid or slurry. The following example illustrates a typical use of theparallel reactor 10.

[0204]FIG. 1 illustrates the configuration of the parallel reactorsystem 10 that could be used for this example 1, with the followingexceptions: the reactor system 10 could be assembled using the staticpressure manifold bar 700 and the blank injection manifold 54.

[0205] To set up the experiment, clean each component comprising thereactor system 10 with tetrahydrofuran (THF) and replace O-ring sealsand stirring blades 40. Attach the static pressure manifold 700 to thereactor block such that the flow path 21 a is coupled to a commonpressure source—Hydrogen gas. The remaining flow paths 20 a, 20 b and 21b are plugged. The stir top assembly 26 is set up using the blankmanifold assembly 54; therefore, no additional chemistry or otherreagents can be introduced into the respective vessels 16 during theexperiment.

[0206] To prepare the chemistry to be evaluated, add approximately 5.0ml of THF containing 50.0 mg of fine powder catalyst of including 10 wt.% Palladium metal supported on activated Carbon and 100 mg of2-ethyl-6-methyl-N-(1-methoxy-2-propylidene) aniline, the startingmaterial, to eight glass vessels 16. Place the vessels 16 in arespective well 14 of the reactor block 12. Once the vessels 16 havebeen added to the reactor wells 14, lower the stir top assembly 26 ontothe reactor block 12 and tighten all head bolts.

[0207] Next, fill and vent the each well 14 with approximately 25 psi ofHydrogen. Repeat the fill and vent sequence four times. This actionpurges the respective reactor wells 14, removing all or substantiallyall of the air from each well 14.

[0208] After the fill and vent sequence, pressurize the respectivereactor wells 14 to 1000 psi using Hydrogen and then activate thestirring blade assembly 30 to mix agitate reaction mixtures at 600 rpm.Set the temperature of each well 14 as follows: TABLE 1 Reactor well 14Temperature (C.) 1 30 2 35 3 40 4 45 5 50 6 55 7 60 8 65

[0209] When the temperature at each well 14 stabilizes, continue to mixor agitate the reaction mixtures for 48 hours at 600 rpm. During thecourse of the 48-hour period withdraw samples from the reactor 10 at thefollowing hourly intervals, while maintaining the temperature andpressure of each vessel: 2, 4, 6, 12, 24, 36, and 48.

[0210] Each sample withdrawn from the respective wells 14 can beanalyzed using gas chromatography to ascertain the effect of temperatureon the reactions, e.g., each sample can be evaluated to ascertain thequantity of the final product,N-(1-methoxy-2-propyl)-2-ethyl-6-methylaniline, produced during theexperiment.

[0211] To end the experiment, reduce the temperature of each well 14 to25° C. and slowly vent the reactor block 12 through the openings 21 a.Once the parallel reactor 10 has been vented, the stir top assembly 26can be removed and the parallel reactor 10 cleaned using an appropriatesolvent.

[0212] This experiment permits the chemist to examine the effect oftemperature on identical reaction mixtures. Using this information, thechemist can determine optimum thermal conditions for reactions utilizingthe reaction mixture or a particular catalyst.

[0213] If desired, the parallel reactor 10 could be set up using theflow through manifold so as to permit the continuous or semi-continuousintroduction of additional chemistry into the reactor wells 14.Additionally, the stir top assembly 26 could be set up using theinjector manifold 46 to permit even more chemistry to be added to eachreactor well 14.

EXAMPLE 2 Method of Using Parallel Reactor 10

[0214] This illustrative example describes how the parallel reactor 10can be used to screen, characterize or evaluate various material andthermal properties, including, but not limited to, molecular weight,specific gravity, elasticity, dielectric constant, conductivity orcalorimetric data.

Reactor Block Assembly Set-up

[0215]FIG. 1 illustrates an embodiment of a parallel reactor assemblythat can be used to perform the following screening of variousmaterials. The parallel reactor can include eight reactor wells, eachwell supporting a removable vessel that prevents direct contact of thereaction mixture with the well 14.

[0216] In this illustrative experiment, the reactor assembly alsoincludes a stir top assembly supporting a stirring blade assembly formixing the reaction mixtures, a pair of dip tubes and a blank injectionmanifold. The reactor assembly also includes a heater and motor controlbox assembly for controlling the temperature of each reactor well andthe operation of the motor controlling the stirring blade assembly.

[0217] Eight different reaction mixtures can be manually loaded intoeach of the vessels 16. The reactor wells 14 can be pressurized in themanner described in Example 1. At any point during the experiment, asmall sample of the reaction mixture in each vessel 16 can be removedand independently analyzed.

A Method of Using Parallel Reactor 10

[0218] A method of processing multiple reaction mixtures using thereactor 10 in can include the steps of (1) providing interchangeablemanifolds having inlet/outlet ports in fluid communication with therespective reactor wells, wherein a fluid can be introduced into,withdrawn from or vented through the respective reactor wells; and (2)evaluating one or more properties of the reaction mixtures or a portionof the reaction mixture by measuring at least one characteristic of thereaction mixtures during at least a portion of the reaction.Additionally, the method could include the step of sampling a portion ofthe reaction mixture from the respective reactor wells via at least oneof the interchangeable manifolds, wherein sampling occurs at a pressuregreater than ambient conditions and without reducing the pressure in therespective reactor wells. And the step of providing the reactor wellswith starting mixtures can be performed by a robotic materials handlingsystem or the starting materials could be manually added to therespective reactor wells.

[0219] Additionally the parallel reactor 10 can be set up to include thefurther steps of: (1) applying a positive pressure to the respectivereactor wells, wherein and the maximum pressure can reach 1500 psi and(2) introducing a fluid or additional chemistry into the respectivereactor wells under pressure.

[0220] The versatility of the parallel reactor 10 permits the reactor 10to be set up to include the additional step of venting outlet portsassociated with the respective reactor wells to a head space defined bythe reactor wells. And the further step of providing an inlet port influid communication with the respective reactor wells so as to establisha common flow path to the respective reactor wells, wherein the methodof using the parallel reactor 10 can include the further steps of (1)providing an outlet port in fluid communication with the respectivereactor wells so as to vent the respective reactor wells to a head spacedefined by the respective reactor wells or plugging said outlet port toprevent fluid flow therethrough; (2) coupling the respective reactorwells to a common pressure source so as to establish a common pressureacross the respective reactor wells.

[0221] Where a common pressure has been established across therespective reactor wells the method of use can include the additionalstep of providing an outlet port in fluid communication with therespective reactor wells so as to vent the respective reactor wells to ahead space defined by the respective reactor wells or plugging saidoutlet port to prevent fluid flow therethrough.

[0222] The property evaluated during the evaluation step can includemolecular weight, specific gravity, elasticity, dielectric constant,conductivity or calorimetric data. The evaluation step can be carriedout by monitoring the temperature of each reaction mixture or bymonitoring heat transfer rates into or out of the respective reactorwells. Monitoring the heat transfer rates into or out of the reactorwells can include the steps of: (1) measuring temperature differencesbetween each of the reaction mixtures and a thermal reservoirsurrounding the reactor wells; and (2) determining heat transfer ratesfrom a calibration relating the temperature differences to heat transferrates.

[0223] The heat transfer rates observed during the monitoring step canbe used to compute the conversion of the starting materials. And therates of reaction can be determined using the conversion of startingmaterials information. In particular, the end point of the reaction canbe easily detected due to the absence of either endothermic orexothermic characteristics in the reaction mixture. The end point of thereaction can be determined using data concerning the consumption of thestarting materials.

[0224] During the experiment, the reaction mixtures can be agitated by(1) bringing a stirring blade assembly into contact with the reactionmixtures, the stirring blade assembly including a spindle supporting arotatable stirring blade; and (2) rotating each of the stirring bladesso as to cause agitation or mixing of the reaction mixtures. Aspreviously discussed, the stirring blade assembly 30 is rotated by amotor 19 driven gear drive system. And the power needed to rotate eachof the stirring members during the rotating step can provide a basis forevaluating the reaction mixtures.

[0225] The reaction mixtures can also be evaluated by monitoring thetorque needed to rotate the stirring blade assembly 30. The torquesupplied to the stirring blade assembly 30 can be monitored by measuringthe phase lag between the torque and the stirring blade assembly 30.

[0226] Additionally, the torque can be a basis for evaluating thereaction mixtures by determining the viscosity of each of the reactionmixtures using a calibration relating torque and viscosity or power andviscosity, where power is the amount of energy required to drive thestirring blade assembly 30. This method of evaluating the reactionmixtures can include the steps of (1) measuring the heat transfer ratesinto or out of the vessels; (2) computing the conversion of the startingmaterials based on heat transfer into or out of the vessels; and (3)calculating the molecular weight of a component of the reaction mixturesbased on conversion of the starting materials and the viscosity of eachof the reaction mixtures.

[0227] Another method for evaluating the reaction mixtures can includethe steps of (1) measuring the heat transfer rates into or out of thevessels 16; (2) computing conversion of the starting materials based onheat transfer rates into or out of the vessels 16; and (3) calculatingmolecular weight of a component of the reaction mixtures based onconversion of the starting materials and on viscosity of each of thereaction mixtures.

[0228] An advantage of the parallel reactor assembly is the ability toremove a portion of the reaction mixture from the respective reactorwells. The removal step can include the further step of removing aportion of the reaction mixture from the respective reactor wellsincludes the further step of establishing a fluid flow path in fluidcommunication with the respective reactor wells and ambient conditions,wherein a portion of the reaction mixture can be forced out of therespective reactor wells and into a sample loop when the fluid flow pathis exposed to ambient conditions.

[0229] The method of removing a portion of the reaction mixture fromrespective reactor well can further include the steps of (1) providingfirst flow control valves having an inlet port supporting a firsttubular member, the first tubular member having one end in fluidcommunication with the respective reactor wells and a second endsupported by the first flow control valve such that the second end canbe exposed to ambient conditions, whereby the back pressure in therespective reactor wells pushes a portion of the reaction mixture intothe first tubular member when the second end of the tubular member isexposed to ambient conditions; (2) providing a second tubular memberhaving one end in fluid communication with the first flow control valveand a second end in fluid communication with a selectively openable andcloseable inlet port of a second flow control valve, wherein the portionof the reaction mixture drawn into the first tubular member can flowthrough the second tubular member, through the second flow control valvevia an inlet/outlet port of the second flow control valve and into thesample loop, said sample loop having one end supported by theinlet/outlet port and an opposite end supported by a third flow controlvalve; (3) providing a fourth tubular member in fluid communication withthe second flow control valve and a sample vial, the fourth tubularmember having a first end in fluid communication with a selectivelyopenable and closeable outlet port defined by the second flow controlvalve and a second end in fluid communication with the sample vial,wherein the portion of the reaction mixture drawn into the sample loopcan flow back through the second flow control, through the fourthtubular member and into the sample vial when the outlet port of thesecond flow control valve is opened; and (4) providing a fifth tubularmember having one end in fluid communication with a selectively openableand closeable inlet port defined by the third flow control valve and asecond end in fluid communication with a supply of pressurized fluid,wherein the pressurized fluid can be caused to flow through the thirdflow control valve, the second flow control valve, the sample loop andthe fourth tubular member upon opening the inlet port of the third flowcontrol valve, closing the inlet port of the second flow control valveand opening a flow path between the sample loop and the sample vial andopening the second inlet port of the second flow control valve.

[0230] In an alternative method of using the parallel reactor system 10,the step of providing the reactor well with starting materials caninclude the step of providing starting materials in the form of aliquid, solid or slurry. Further still, the step of providing thereactor wells with starting materials can include the step of adding aheterogeneous, homogeneous or asymmetric catalyst to the startingmaterials. Even further still, the step of providing can include thestep of providing starting materials for conducting polymerization orhydrogenation reactions.

[0231] Alternatively, if the parallel reactor 10 is placed in thechamber 100, as previously discussed, the step of providing the startingmixtures to the respective chambers could include the additional step ofblanketing the reactor wells in an inert gas atmosphere while providingthe respective reactor wells with the starting materials.

[0232] Preferred embodiments of the present invention have beendisclosed. The explanations and illustrations presented herein areintended to acquaint others skilled in the art with the invention, itsprinciples, and its practical application. A person of ordinary skill inthe art would realize, however, that certain modifications would comewithin the teachings of this invention. Therefore, the following claimsshould be studied to determine the true scope and content of theinvention.

What is claimed is:
 1. An apparatus for parallel processing of reactionmixtures comprising: a reactor block including reaction chambers forcontaining reaction mixtures under pressure, the reactor block furtherincluding a first sidewall, a second sidewall, and a first plurality offluid flow paths providing fluid communication with the first sidewalland respective reaction chambers and the second sidewall and respectivereaction chambers; a stirring system including a base plate defining asecond plurality of flow paths, wherein respective flow paths of saidsecond plurality of flow paths are in fluid communication withrespective reaction chambers and respective fluid flow paths of saidfirst plurality of flow paths, and said base plate supporting aplurality of stirring blade assemblies for mixing the reaction mixtures,wherein one stirring blade assembly of said plurality of stirring bladeassemblies is received in the respective reaction chambers; andinterchangeable manifolds supported by the first sidewall and the secondsidewall, the interchangeable manifolds defining a plurality of manifoldinlet/outlet ports, wherein respective inlet/outlet ports of saidplurality of inlet/outlet ports are in communication with respectivefluid flow paths of said first plurality of fluid flow paths and permitfluid to be introduced into or vented from the respective reactionchambers.
 2. The apparatus of claim 1, wherein a group of four fluidflow paths of the first plurality of fluid flow paths are in fluidcommunication with respective reaction chambers.
 3. The apparatus ofclaim 2, wherein two of the four fluid flow paths are defined by thefirst sidewall and two of the four fluid flow paths are defined by thesecond sidewall.
 4. The apparatus of claim 3, wherein one of the twofluid flow paths defined by the first sidewall is in fluid communicationwith the respective reaction chamber via one flow path of said secondplurality of flow paths, and one of the two fluid flow paths defined bythe second sidewall is in fluid communication with the respectivereaction chamber via one flow path of said second plurality of flowpaths.
 5. The apparatus of claim 3, wherein one of the two fluid flowpaths defined by the first sidewall is in fluid communication with ahead space defined by the respective reaction chambers above thereaction mixture via one flow path of said first plurality of fluid flowpaths, and one of the two fluid flow paths defined by the secondsidewall is in fluid communication with the head space of the respectivereaction chamber via one flow path of said first plurality of fluid flowpaths.
 6. The apparatus of claim 1, wherein the respective reactorchambers define a reactor well having an open center.
 7. The apparatusof claim 6, wherein the open center of each reactor well receives avessel for retaining the reaction mixture.
 8. The apparatus of claim 7,wherein the vessels are removable liners, each liner having an interiorsurface defining a cavity for containing one of the reaction mixturesand an exterior surface dimensioned so that the liners fit within onereactor well.
 9. The apparatus of claim 6, wherein the removable linersare glass or plastic vials.
 10. The apparatus of claim 1, wherein theplurality of inlet/outlet ports of the interchangeable manifolds defineseparate flow paths through the respective interchangeable manifoldbars.
 11. The apparatus of claim 10, wherein a first group ofinlet/outlet ports of said plurality of inlet/outlet ports includesinlet/outlet ports in fluid communication with respective flow paths ofsaid first plurality of flow paths and respective flow paths of saidsecond plurality of flow paths, wherein each inlet/outlet port of saidfirst group is in fluid communication with respective flow paths of saidfirst plurality of fluid flow paths and respective flow paths of saidsecond plurality of fluid flow paths.
 12. The apparatus of claim 1,wherein a second group of inlet/outlet ports selected from saidplurality of inlet/outlet ports are in fluid communication withrespective flow paths of said first plurality of fluid flow paths,wherein the respective flow paths of said first plurality of fluid flowpaths is in fluid communication with a head space defined within therespective reaction chambers, wherein each inlet/outlet port of saidsecond group is in fluid communication with a respective flow path ofsaid first plurality of fluid flow paths.
 13. The apparatus of claim 12,wherein a third group of inlet/outlet ports selected from said pluralityof inlet/outlet ports is in fluid communication with a source of fluidto be introduced into the respective reaction chambers, wherein eachinlet/outlet port of said third group establishes separate fluid flowpaths with a respective flow path of said first plurality of fluid flowpaths.
 14. The apparatus of claim 13, wherein a fourth group ofinlet/outlet ports selected from said plurality of inlet/outlet ports isvented to the head space, wherein each inlet/outlet port of said fourthgroup establishes separate fluid flow paths with a respective flow pathof said first plurality of fluid flow paths.
 15. The apparatus of claim1, wherein the interchangeable manifolds include a manifold bar whereina fifth group of inlet/outlet ports selected from said plurality ofinlet/outlet ports are coupled in fluid communication so as to define acommon flow path through the fifth group, wherein each inlet/outlet portof said fifth group is in fluid communication with separate flow pathsforming said first plurality of fluid flow paths.
 16. The apparatus ofclaim 15, wherein said fifth group is coupled to a common fluid sourceso as to form a common flow path therethrough.
 17. The apparatus ofclaim 16, wherein each inlet/outlet port comprising the fifth group ofinlet/outlet ports is in fluid communication with the respectivereaction chambers.
 18. The apparatus of claim 15, wherein the fifthgroup of inlet/outlet ports is coupled to a common pressure source so asto form a common flow path therethrough.
 19. The apparatus of claim 18,wherein each inlet/outlet port of the fifth group of inlet/outlet portsis vented to a head space defined by the respective reaction chambers.20. The apparatus of claim 10, 16, or 18, wherein one of saidinterchangeable manifold bars is supported by the first sidewall and thesecond sidewall respectively.
 21. The apparatus of claim 1, wherein eachstirring blade assembly includes: a spindle, each spindle having a firstend and a second end; and a stirring blade attached to the first end ofthe spindle.
 22. The apparatus of claim 21, wherein the second end ofthe spindle is mechanically coupled to a drive mechanism.
 23. Theapparatus of claim 22, wherein the drive mechanism is a motor drivengear drive system.
 24. The apparatus of claim 23, further including amotor speed control electrically coupled to the motor for controlling ormonitoring the rotational speed of the motor.
 25. The apparatus of claim23, wherein the drive mechanism is enclosed by a cover.
 26. Theapparatus of 25, wherein the cover is metal.
 27. The apparatus of claim1, wherein the stirring system base plate provides a sealing surface forisolating the reaction chambers from ambient conditions, and furtherpermitting the application of a positive pressure to the respectivereaction chambers, wherein the maximum pressure can reach 1500 psi. 28.The apparatus of claim 1, wherein the stirring system supports aninjector system for introducing additional chemistry into the respectivereaction chambers under pressure, the injector system including aninjector manifold bar defining a plurality of injector manifoldinlet/outlet ports for receiving a vessel coupling the injector manifoldbar to a source of injection fluid, wherein separate injector manifoldinlet/outlet ports forming said plurality of injector inlet/outlet portsis in fluid communication with the respective reaction chambers.
 29. Theapparatus of claim 28 further including a third plurality of flow pathsdefined by the injector manifold bar, wherein separate flow paths ofsaid third plurality flow paths are in fluid communication with therespective reaction chambers via one flow path of a fourth plurality offlow paths defined by the base plate.
 30. The apparatus of claim 29,wherein the respective flow paths comprising the fourth plurality offlow paths are separately coupled in fluid communication with a deliverytube, wherein separate delivery tubes are in fluid communication witheach of the respective chambers.
 31. The apparatus of claim 28, whereinthe injector system further includes separate fill ports received in therespective injector manifold inlet/outlet ports and a separate fluiddelivery probe supported by the respective fill ports, wherein eachdelivery probe is in fluid communication with chemistry or othercomponents to be injected into the respective reaction chambers.
 32. Theapparatus of claim 31, wherein the respective fill ports include anelongated body having a longitudinal axis and a bore centered on thelongitudinal axis, the bore extending the length of the elongated body.33. The apparatus of claim 32 further including a fitting received withthe bore of the respective fill ports for supporting the delivery probe.34. The apparatus of claim 33, wherein the fitting is made of achemically resistant plastic material.
 35. The apparatus of claim 1,including a sampling manifold assembly coupled in fluid communicationwith the respective reaction chambers via at least one of theinterchangeable manifolds, wherein a portion of the reaction mixtureretained in the respective reaction chambers can be withdrawn from therespective reaction chamber through respective fluid flow paths of saidfirst plurality of fluid flow paths, respective flow paths of saidsecond plurality of flow paths, or both, without depressurizing orlowering the pressure in the respective reaction chambers.
 36. Theapparatus of claim 35, wherein the sampling manifold assembly includes:first flow control valves having an inlet port and an outlet port,wherein separate flow control valves are in fluid communication with oneof the respective reaction chambers; second flow control valves, whereineach respective second flow control valve includes one inlet port, oneinlet/outlet port and one outlet port, wherein separate inlet ports arein fluid communication with separate valves of said first flow controlvalves; and third flow control valves, wherein each respective thirdflow control includes one inlet port and one outlet port, whereinseparate inlet ports are in fluid communication with separate secondflow control valves and separate outlet ports are in fluid communicationwith a pressure source.
 37. The apparatus of claim 35, wherein the firstflow control valves include: a first tubular member having a first endcoupled to the inlet port defined by the first flow control valve and asecond end in fluid communication with one of the respective reactionchambers, and a second tubular member having one end supported by theoutlet port of the first flow control valve and a second end coupled tothe first inlet port of one value of said second flow control valves.38. The apparatus of claim 37, wherein the second end of separate firsttubular members are in fluid communication with a dip tube selected froma plurality of dip tubes, each dip tube having one end supported by aportion of the stirring system so as to establish fluid communicationbetween one dip tube and one flow path of said second plurality of flowpaths and an opposite end that extends at least partially into one ofthe respective reaction chambers.
 39. The apparatus of claim 38, whereinthe respective dip tubes are hollow tubular members.
 40. The apparatusof claim 39, wherein the dip tubes can be glass or plastic vials orliners or Teflon® tubes.
 41. The apparatus of claim 37, wherein theseparate inlet/outlet ports of the respective second flow control valvessupports a third tubular member, wherein one end of the third tubularmember is supported by the inlet/outlet port of the respective secondflow control valves and an opposite end of the third tubular member issupported by the outlet port of the third flow control valves, and theoutlet ports of the respective second flow control valves support afourth tubular member having one end coupled to the outlet port of oneof the respective second flow control valves and a second end in fluidcommunication with a sample vial.
 42. The apparatus of claim 41, whereinthe inlet ports of the respective third flow control valves support afifth tubular member coupled to a pressure source, and the third flowcontrol valves include further an outlet port in fluid communicationwith the inlet/outlet port of the second flow control valve.
 43. Theapparatus of claim 1, further including temperature control systems formaintaining the reaction mixture contained in the respective reactionchambers at a desired temperature.
 44. The apparatus of claim 43,wherein the respective temperature control systems include: one or moreheating devices in thermal contact with respective reaction chambers,wherein the respective reaction chambers can be heated to the same ordifferent temperatures; and temperature sensors in thermal contact withthe respective reaction chambers for measuring the temperature of therespective reaction mixture, the respective reaction chamber or both.45. The apparatus of claim 44, wherein the temperature sensors arethermocouples.
 46. The apparatus of claim 44, wherein the respectivetemperature control systems further include a microprocessor formonitoring or adjusting the temperature of the heating device.
 47. Theapparatus of claim 46, wherein the respective microprocessor iselectrically coupled to a solid state relay for controlling power to therespective heating devices, wherein the solid state relay can be causedto become active if the respective microprocessor senses a temperaturein the respective reaction chamber above or below a preselected ordesired value.
 48. The apparatus of claim 43, wherein the temperaturecontrol systems further include separate display screens for displayingthe temperature of the respective reaction chambers or informationdeterminative of the temperature of the respective reaction chamber. 49.The apparatus of claim 48, wherein the respective display screenssupport a selectively adjustable temperature control switch for varyingthe temperature of the respective heating devices.
 50. The apparatus ofclaim 1, wherein the reaction chambers are continuous or semi-continuousflow reaction chambers.
 51. The apparatus of claim 1 further including afilter for filtering the fluid introduced into, withdrawn or ventedfrom, the respective reaction chambers.
 52. An apparatus for parallelprocessing of reaction mixtures comprising: a reactor block includingreaction chambers for containing reaction mixtures under pressure, thereactor block further including a first sidewall, a second sidewall, anda first plurality of fluid flow paths providing fluid communication withthe first sidewall and respective reaction chambers and the secondsidewall and respective reaction chambers; a stirring system including abase plate defining a second plurality of flow paths, wherein respectiveflow paths of said second plurality of flow paths are in fluidcommunication with respective reaction chambers and respective fluidflow paths of said first plurality of flow paths, and said base platesupporting a plurality of stirring blade assemblies for mixing thereaction mixtures, wherein one stirring blade assembly of said pluralityof stirring blade assemblies is received in the respective reactionchambers; at least one interchangeable manifold supported by the firstsidewall, the interchangeable manifold defining a plurality of manifoldinlet/outlet ports, wherein respective inlet/outlet ports of saidplurality of inlet/outlet ports are in communication with respectivefluid flow paths of said first plurality of fluid flow paths; and asampling manifold assembly supported by the second sidewall in fluidcommunication with the respective reaction chambers through respectiveflow paths of the first plurality of flow paths, the second plurality offlow paths or both, wherein a portion of the mixtures can be withdrawnfrom the respective reaction chambers without depressurizing or loweringthe pressure in the respective reaction chambers.
 53. The apparatus ofclaim 52, wherein the sampling manifold assembly includes: first flowcontrol valves having an inlet port and an outlet port, wherein separateflow control valves are in fluid communication with one of therespective reaction chambers; second flow control valves, wherein eachrespective second flow control valve includes one inlet port, oneinlet/outlet port and one outlet port, wherein separate inlet ports arein fluid communication with separate valves of said first flow controlvalves; and third flow control valves, wherein each respective thirdflow control includes one inlet port and one outlet port, whereinseparate inlet ports are in fluid communication with separate secondflow control valves and separate outlet ports are in fluid communicationwith a pressure source.
 54. The apparatus of claim 52, wherein the firstflow control valves include: a first tubular member having a first endcoupled to the inlet port defined by the first flow control valve and asecond end in fluid communication with one of the respective reactionchambers, and a second tubular member having one end supported by theoutlet port of the first flow control valve and a second end coupled tothe first inlet port of one value of said second flow control valves.55. The apparatus of claim 54, wherein the second end of separate firsttubular members are in fluid communication with a dip tube selected froma plurality of dip tubes, each dip tube having one end supported by aportion of the stirring system so as to establish fluid communicationbetween one dip tube and one flow path of said second plurality of flowpaths and an opposite end that extends at least partially into one ofthe respective reaction chambers.
 56. The apparatus of claim 55, whereinthe respective dip tubes are hollow tubular members.
 57. The apparatusof claim 56, wherein the dip tubes can be glass or plastic vials orliners or Teflon® tubes.
 58. The apparatus of claim 54, wherein theseparate inlet/outlet ports of the respective second flow control valvessupports a third tubular member, wherein one end of the third tubularmember is supported by the inlet/outlet port of the respective secondflow control valves and an opposite end of the third tubular member issupported by the outlet port of the third flow control valves, and theoutlet ports of the respective second flow control valves support afourth tubular member having one end coupled to the outlet port of oneof the respective second flow control valves and a second end in fluidcommunication with a sample vial.
 59. The apparatus of claim 58, whereinthe inlet ports of the respective third flow control valves support afifth tubular member coupled to a pressure source, and the third flowcontrol valves include further an outlet port in fluid communicationwith the inlet/outlet port of the second flow control valve.
 60. Anapparatus for parallel processing of reaction mixtures comprising: areactor block including reaction chambers for containing reactionmixtures under pressure, the reactor block further including a firstsidewall, a second sidewall, and a first plurality of fluid flow pathsproviding fluid communication with the first sidewall and respectivereaction chambers and the second sidewall and respective reactionchambers; a stirring system including a base plate defining a secondplurality of flow paths, wherein at least respective flow paths of saidsecond plurality of flow paths are in fluid communication withrespective reaction chambers, respective fluid flow paths of said firstplurality of flow paths or both, and said base plate supporting aplurality of stirring blade assemblies for mixing the reaction mixtures,wherein one stirring blade assembly of said plurality of stirring bladeassemblies is received in one of the respective reaction chambers, andsaid base plate further providing a sealing surface for isolating thereaction chambers from ambient conditions, and further permittingapplying a positive pressure to the respective reaction chambers,wherein the maximum pressure can reach 1500 psi; interchangeablemanifolds supported by the first sidewall and the second sidewall forallowing the introduction of a fluid into or withdrawing a fluid fromthe respective reaction chambers, wherein said introduction orwithdrawal of fluid occurs under pressure and without depressurizing orreducing the pressure of the respective reaction chambers, theinterchangeable manifolds also defining a plurality of manifoldinlet/outlet ports, wherein respective inlet/outlet ports of saidplurality of inlet/outlet ports are in communication with respectivefluid flow paths of said first plurality of fluid flow paths; and asampling manifold assembly coupled in fluid communication with theinterchangeable manifolds, wherein a portion of the reaction mixtureretained in the respective reaction chambers can be withdrawn from therespective reaction chambers through respective fluid flow paths of saidfirst plurality of fluid flow paths and respective flow paths of saidsecond plurality of flow paths, or both, without depressurizing therespective reaction chamber.
 61. The apparatus of claim 60, wherein agroup of four fluid flow paths of the first plurality of fluid flowpaths are in fluid communication with respective reaction chambers. 62.The apparatus of claim 61, wherein two of the four fluid flow paths aredefined by the first sidewall and two of the four fluid flow paths aredefined by the second sidewall.
 63. The apparatus of claim 62, whereinone of the two fluid flow paths defined by the first sidewall is influid communication with one reaction chamber of the respective reactionchambers via one flow path of said second plurality of flow paths, andone of the two fluid flow paths defined by the second sidewall is influid communication with one reaction chamber of the respective reactionchambers via one flow path of said second plurality of flow paths. 64.The apparatus of claim 62, wherein one of the two fluid flow pathsdefined by the first sidewall is in fluid communication with a headspace defined by one reaction chamber of the respective reactionchambers above the reaction mixture via one flow path of said firstplurality of fluid flow paths, and one of the two fluid flow pathsdefined by the second sidewall is in fluid communication with the headspace of one reaction chamber of the respective reaction chamber via oneflow path of said first plurality of fluid flow paths.
 65. The apparatusof claim 60, wherein the respective reactor chambers define a reactorwell having an open center.
 66. The apparatus of claim 65, wherein theopen center of each reactor well receives a vessel for retaining thereaction mixture.
 67. The apparatus of claim 66, wherein the vessels areremovable liners, each liner having an interior surface defining acavity for containing one of the reaction mixtures and an exteriorsurface dimensioned so that the liners fit within one reactor well. 68.The apparatus of claim 65, wherein the removable liners are glass orplastic vials.
 69. The apparatus of claim 60, wherein the plurality ofinlet/outlet ports of the interchangeable manifolds define separate flowpaths through the respective interchangeable manifold bars.
 70. Theapparatus of claim 69, wherein a first group of inlet/outlet ports ofsaid plurality of inlet/outlet ports having inlet/outlet ports in fluidcommunication with respective flow paths of said first plurality of flowpaths and respective flow paths of said second plurality of flow paths,wherein each inlet/outlet port of said first group establishes separatefluid flow paths with a respective flow path of said plurality of fluidflow paths.
 71. The apparatus of claim 70, wherein a second group ofinlet/outlet ports selected from said plurality of inlet/outlet portsinclude inlet/outlet ports in fluid communication with respective flowpaths of said first plurality of fluid flow paths, wherein respectiveflow paths of said first plurality of fluid flow paths are in fluidcommunication with a head space defined within the respective reactionchambers, wherein respective inlet/outlet ports of said second group arein fluid communication with respective flow paths of said firstplurality of fluid flow paths.
 72. The apparatus of claim 71, wherein athird group of inlet/outlet ports selected from said plurality ofinlet/outlet ports includes inlet/outlet ports in fluid communicationwith a source of fluid to be introduced into the respective reactionchambers, wherein each inlet/outlet port of said third group establishesfluid flow paths with one flow path of said first plurality of fluidflow paths.
 73. The apparatus of claim 72, wherein a fourth group ofinlet/outlet ports selected from said plurality of inlet/outlet ports isvented to the head space, wherein each inlet/outlet port of said fourthgroup is in fluid communication with respective fluid flow paths of saidfirst plurality of fluid flow paths.
 74. The apparatus of claim 73,wherein the interchangeable manifolds include a manifold bar wherein afifth group of inlet/outlet ports selected from said plurality ofinlet/outlet ports is coupled in fluid communication so as to define acommon flow path through each inlet/outlet port of said fifth group,wherein each inlet/outlet port of said fifth group establishes fluidflow paths with respective flow paths of said first plurality of fluidflow paths.
 75. The apparatus of claim 74, wherein said fifth group iscoupled to a common fluid source so as to form a common flow paththerethrough.
 76. The apparatus of claim 75, wherein each inlet/outletport comprising the fifth selected group of inlet/outlet ports is influid communication with the respective reactor wells.
 77. The apparatusof claim 74, wherein each inlet/outlet port of the fifth selected groupof inlet/outlet ports is coupled to a common pressure source so as toform a common flow path therethrough.
 78. The apparatus of claim 77,wherein each inlet/outlet port of the fifth selected group ofinlet/outlet ports is vented to a head space defined by the respectivechambers.
 79. The apparatus of claim 69, 75, or 77, wherein one of saidinterchangeable manifold bars is supported by the first sidewall and thesecond sidewall respectively.
 80. The apparatus of claim 60, whereineach stirring blade assembly includes: a spindle, each spindle having afirst end and a second end; and a stirring blade attached to the firstend of the spindle.
 81. The apparatus of claim 80, wherein the secondend of the spindle is mechanically coupled to a drive mechanism.
 82. Theapparatus of claim 81, wherein the drive mechanism is a motor drivengear drive system.
 83. The apparatus of claim 82, further including amotor speed control electrically coupled to the motor for controlling ormonitoring the rotational speed of the motor.
 84. The apparatus of claim82, wherein the drive mechanism is enclosed by a cover.
 85. Theapparatus of 84, wherein the cover is metal.
 86. The apparatus of claim60, wherein the stirring system supports an injector system forintroducing additional chemistry into the respective reaction chambersunder pressure, the injector system including an injector manifold bardefining a plurality of injector manifold inlet/outlet ports forreceiving a vessel coupling the injector manifold bar to a source ofinjection fluid, wherein separate injector manifold inlet/outlet portsforming said plurality of injector inlet/outlet ports is in fluidcommunication with the respective reaction chambers.
 87. The apparatusof claim 60 further including a third plurality of flow paths defined bythe injector manifold bar, wherein separate flow paths of said thirdplurality flow paths are in fluid communication with the respectivereaction chambers via one flow path of a fourth plurality of flow pathsdefined by the base plate.
 88. The apparatus of claim 87, wherein therespective flow paths comprising the fourth plurality of flow paths areseparately coupled in fluid communication with a delivery tube, whereinseparate delivery tubes are in fluid communication with each of therespective chambers.
 89. The apparatus of claim 87, wherein the injectorsystem further includes separate fill ports received in the respectiveinjector manifold inlet/outlet ports and a separate fluid delivery probesupported by the respective fill ports, wherein each delivery probe isin fluid communication with chemistry or other components to be injectedinto the respective reaction chambers.
 90. The apparatus of claim 89,wherein the respective fill ports include an elongated body having alongitudinal axis and a bore centered on the longitudinal axis, the boreextending the length of the elongated body.
 91. The apparatus of claim90 further including a fitting received with the bore of the respectivefill ports for supporting the delivery probe.
 92. The apparatus of claim92, wherein the fitting is made of a chemically resistant plasticmaterial.
 93. The apparatus of claim 60, wherein the sampling manifoldassembly includes: first flow control valves having an inlet port and anoutlet port, wherein separate flow control valves are in fluidcommunication with one of the respective reaction chambers; second flowcontrol valves, wherein each respective second flow control valveincludes one inlet port, one inlet/outlet port and one outlet port,wherein separate inlet ports are in fluid communication with separatevalves of said first flow control valves; and third flow control valves,wherein each respective third flow control includes one inlet port andone outlet port, wherein separate inlet ports are in fluid communicationwith separate second flow control valves and separate outlet ports arein fluid communication with a pressure source.
 94. The apparatus ofclaim 93, wherein the first flow control valves include: a first tubularmember having a first end coupled to the inlet port defined by the firstflow control valve and a second end in fluid communication with one ofthe respective reaction chambers, and a second tubular member having oneend supported by the outlet port of the first flow control valve and asecond end coupled to the first inlet port of one value of said secondflow control valves.
 95. The apparatus of claim 94, wherein the secondend of separate first tubular members are in fluid communication with adip tube selected from a plurality of dip tubes, each dip tube havingone end supported by a portion of the stirring system so as to establishfluid communication between one dip tube and one flow path of saidsecond plurality of flow paths and an opposite end that extends at leastpartially into one of the respective reaction chambers.
 96. Theapparatus of claim 95, wherein the respective dip tubes are hollowtubular members.
 97. The apparatus of claim 96, wherein the dip tubescan be glass or plastic vials or liners or Teflon® tubes.
 98. Theapparatus of claim 95, wherein the separate inlet/outlet ports of therespective second flow control valves supports a third tubular member,wherein one end of the third tubular member is supported by theinlet/outlet port of the respective second flow control valves and anopposite end of the third tubular member is supported by the outlet portof the third flow control valves, and the outlet ports of the respectivesecond flow control valves support a fourth tubular member having oneend coupled to the outlet port of one of the respective second flowcontrol valves and a second end in fluid communication with a samplevial.
 99. The apparatus of claim 98, wherein the inlet ports of therespective third flow control valves support a fifth tubular membercoupled to a pressure source, and the third flow control valves includefurther an outlet port in fluid communication with the inlet/outlet portof the second flow control valve.
 100. The apparatus of claim 50,further including temperature control systems for maintaining thereaction mixture contained in the respective reaction chambers at adesired temperature.
 101. The apparatus of claim 100, wherein therespective temperature control systems include: one or more heatingdevices in thermal contact with respective reaction chambers, whereinthe respective reaction chambers can be heated to the same or differenttemperatures; and temperature sensors in thermal contact with therespective reaction chambers for measuring the temperature of therespective reaction mixture, the respective reaction chamber or both.102. The apparatus of claim 101, wherein the temperature sensors arethermocouples.
 103. The apparatus of claim 102, wherein the respectivetemperature control systems further include a microprocessor formonitoring and adjusting the temperature of the heating device.
 104. Theapparatus of claim 103, wherein the respective microprocessor iselectrically coupled to a solid state relay for controlling power to therespective heating devices, wherein the solid state relay can be causedto become active if the respective microprocessor senses a temperaturein the respective reaction chamber above or below a preselected ordesired value.
 105. The apparatus of claim 104, wherein the temperaturecontrol system further includes separate display screens for displayingthe temperature of the respective reaction chambers or informationdeterminative of the temperature of the respective reaction chamber.106. The apparatus of claim 105, wherein the respective display screenssupport a selectively adjustable temperature control switch for varyingthe temperature of the respective heating devices.
 107. The apparatus ofclaim 60, wherein the reaction chambers are continuous orsemi-continuous flow reaction chambers.
 108. The apparatus of claim 60further including a filter for filtering the fluid introduced intowithdrawn or vented from, the respective reaction chambers.
 109. Amethod of parallel processing multiple reaction mixtures comprising thesteps of: providing reaction chambers with starting materials to formreaction mixtures; agitating the reaction mixtures during at least aportion of the experiment; providing interchangeable manifolds havinginlet/outlet ports in fluid communication with the respective reactionchambers, wherein a fluid can be introduced into, withdrawn from orvented through the respective reaction chambers; and evaluating one ormore properties of the reaction mixtures or a portion of the reactionmixture by measuring at least one characteristic of the reactionmixtures during at least a portion of the reaction.
 110. The method ofclaim 109, further including the step of sampling a portion of thereaction mixture from the respective reaction chambers via at least oneof the interchangeable manifolds, wherein sampling occurs at a pressuregreater than ambient conditions and without reducing the pressure in therespective reaction chambers.
 111. The method of claim 109 furtherincluding the step of filtering fluid introduced into or withdrawn fromthe respective reaction chambers.
 112. The method of claim 109 furtherincluding the step of applying a positive pressure to the respectivereaction chambers, wherein the maximum pressure is 1500 psi.
 113. Themethod of claim 109 further including the step of introducing a fluidinto the respective reaction chambers under pressure.
 114. The method ofclaim 113 further including the step of venting outlet ports associatedwith the respective reaction chambers to a head space defined by thereaction chambers.
 115. The method of claim 113 further including thestep of providing an inlet port in fluid communication with therespective reaction chambers so as to establish a common flow path tothe respective reaction chambers.
 116. The method of claim 115 furtherincluding the step of providing an outlet port in fluid communicationwith the respective reaction chambers so as to vent the respectivereaction chambers to a head space defined by the respective reactionchambers or plugging said outlet port to prevent fluid flowtherethrough.
 117. The method of claim 115 further including the step ofcoupling the respective reaction chambers to a common pressure source soas to establish a common pressure across the respective reactionchambers.
 118. The method of claim 117 further including the step ofproviding an outlet port in fluid communication with the respectivereaction chambers so as to vent the respective reaction chambers to ahead space defined by the respective reaction chambers or plugging saidoutlet port to prevent fluid flow therethrough.
 119. The method of claim109, wherein the reaction chambers are provided with starting materialsusing a robotic materials handling system.
 120. The method of claim 119further including the step of placing the reaction chambers in a sealedenclosure.
 121. The method of claim 120 further including the step ofblanketing the respective reaction chambers in an inert gas atmospherewhile providing the respective reaction chambers with the startingmaterials.
 122. The method of claim 109, wherein the reaction mixturesare evaluated by monitoring a temperature of each of the reactionmixtures.
 123. The method of claim 109, wherein the reaction mixturesare evaluated by monitoring heat transfer rates into or out of therespective reaction chambers.
 124. The method of claim 123, whereinmonitoring the heat transfer rates comprises the steps of: measuringtemperature differences between each of the reaction mixtures and athermal reservoir surrounding the reaction chambers; and determiningheat transfer rates from a calibration relating the temperaturedifferences to heat transfer rates.
 125. The method of claim 123 furthercomprising computing conversion of the starting materials based on theheat transfer rates of the monitoring step.
 126. The method of claim125, further comprising determining rates of reaction based onconversion of the starting materials.
 127. The method of claim 109,wherein the agitating step can include the steps of: bringing a stirringblade assembly into contact with the reaction mixtures, the stirringblade assembly including a spindle supporting a rotatable stirringblade; and rotating each of the stirring blades so as to cause agitationor mixing of the reaction mixtures.
 128. The method of claim 109,wherein the stirring blades rotate at the same rate, the stirring bladesbeing driven by a motor driven gear drive system.
 129. The method ofclaim 127, wherein the reaction mixtures are evaluated by monitoring thetorque needed to rotate the stirring blade assembly.
 130. The method ofclaim 129, wherein the torque is monitored by measuring the phase lagbetween the motor torque and the torque of the stirring blade assembly.131. The method of claim 129, wherein the reaction mixtures areevaluated by determining the viscosity of each of the reaction mixturesfrom a calibration relating torque and viscosity.
 132. The method ofclaim 131, wherein the reaction mixtures are evaluated by the steps of:measuring the heat transfer rates into or out of the respective reactionchambers; computing conversion of the starting materials based on heattransfer rates into or out of the respective reaction chambers; andcalculating molecular weight of a component of the reaction mixturesbased on conversion of the starting materials and on viscosity of eachof the reaction mixtures.
 133. The method of claim 127, wherein theevaluating step further comprises the step of monitoring the powerneeded to rotate each of the stirring blade assemblies in the rotatingstep.
 134. The method of claim 133, wherein the reaction mixtures areevaluated by determining the viscosity of each of the reaction mixturesfrom a calibration relating power and viscosity.
 135. The method ofclaim 134, wherein the reaction mixtures are evaluated by the steps of:measuring the heat transfer rates into or out of the respective reactionchambers; computing the conversion of the starting materials based onheat transfer into or out of the reaction chambers; and calculating themolecular weight of a component of the reaction mixtures based onconversion of the starting materials and the viscosity of each of thereaction mixtures.
 136. The method of claim 109, wherein the propertyevaluated during the evaluation step includes molecular weight, specificgravity, elasticity, dielectric constant, conductivity or calorimetricdata.
 137. The method of claim 109, wherein the step of removing aportion of the reaction mixture from the respective reaction chambersincludes the step of establishing a fluid flow path in fluidcommunication with the respective reaction chambers and ambientconditions, wherein a portion of the reaction mixture can be forced outof the respective reaction chambers and into a sample loop when thefluid flow path is exposed to ambient conditions.
 138. The method ofclaim 137, wherein the step of removing a portion of the reactionmixture from the respective reaction chambers further includes the stepof: providing first flow control valves having an inlet port supportinga first tubular member, the first tubular member having one end in fluidcommunication with the respective reaction chambers and a second endsupported by the first flow control valve such that the second end canbe exposed to ambient conditions, whereby the back pressure in therespective reaction chambers pushes a portion of the reaction mixtureinto the first tubular member when the second end of the tubular memberis exposed to ambient conditions.
 139. The method of claim 138, furtherincluding the step of: providing a second tubular member having one endin fluid communication with the first flow control valve and a secondend in fluid communication with a selectively openable and closeableinlet port of a second flow control valve, wherein the portion of thereaction mixture drawn into the first tubular member can flow throughthe second tubular member, through the second flow control valve via aninlet/outlet port of the second flow control valve and into the sampleloop, said sample loop having one end supported by the inlet/outlet portand an opposite end supported by a third flow control valve.
 140. Themethod of claim 139, further including the step of: providing a fourthtubular member in fluid communication with the second flow control valveand a sample vial, the fourth tubular member having a first end in fluidcommunication with a selectively openable and closeable outlet portdefined by the second flow control valve and a second end in fluidcommunication with the sample vial, wherein the portion of the reactionmixture drawn into the sample loop can flow back through the second flowcontrol, through the fourth tubular member and into the sample vial whenthe outlet port of the second flow control valve is opened.
 141. Themethod of claim 140, further including the steps of: providing a fifthtubular member having one end in fluid communication with a selectivelyopenable and closeable inlet port defined by the third flow controlvalve and a second end in fluid communication with a supply ofpressurized fluid, wherein the pressurized fluid can be caused to flowthrough the third flow control valve, the second flow control valve, thesample loop and the fourth tubular member upon opening the inlet port ofthe third flow control valve, closing the inlet port of the second flowcontrol valve and opening a flow path between the sample loop and thesample vial and opening the second inlet port of the second flow controlvalve.
 142. The method of claim 109, wherein the step of providing thereaction chamber with starting materials includes the step of providingstarting materials in the form of a liquid, solid or a slurry.
 143. Themethod of claim 109, wherein the step of providing the reaction chamberswith starting materials can further include the step of adding aheterogeneous, homogeneous or asymmetric catalyst to the startingmaterials.
 144. The method of claim 109, wherein the step of providingcan include the step of providing the reaction chambers with startingmaterials includes the step of providing starting materials forconducting polymerization or hydrogenation reactions.